#------------------------------------------------------------------------------
#$Date: 2018-10-05 04:45:29 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211330 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/16/7231611.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_7231611
loop_
_publ_author_name
'Han, Jingyu'
'Li, Shufen'
'Tang, Chunying'
'Zheng, Wei'
'Jiang, Wenqing'
'Jia, Dingxian'
_publ_section_title
;
 Hydrazine-solvothermal methods to synthesize polymeric thioarsenates from
 one-dimensional chains to a three-dimensional framework
;
_journal_issue                   59
_journal_name_full               'RSC Advances'
_journal_page_first              34078
_journal_paper_doi               10.1039/C8RA06335D
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'As2 H24 Mn3 N8 S8'
_chemical_formula_sum            'As2 H24 Mn3 N8 S8'
_chemical_formula_weight         707.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-07-17 deposited with the CCDC.
2018-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                78.68(3)
_cell_angle_beta                 83.53(3)
_cell_angle_gamma                77.92(3)
_cell_formula_units_Z            1
_cell_length_a                   6.6881(13)
_cell_length_b                   7.9869(16)
_cell_length_c                   10.966(2)
_cell_measurement_reflns_used    3104
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      3.1237
_cell_volume                     560.1(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4629
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    5.343
_exptl_absorpt_correction_T_max  0.4146
_exptl_absorpt_correction_T_min  0.1753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             349
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         2030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0282P)²+0.5550P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0699
_reflns_number_gt                1950
_reflns_number_total             2030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ra06335d2.cif
_cod_data_source_block           compound_6
_cod_original_cell_volume        560.09(19)
_cod_database_code               7231611
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
As1 As 0.27124(5) 0.34611(4) 0.32447(3) 0.01871(11) Uani 1 1 d .
Mn1 Mn 0.23116(8) 0.57228(7) 0.56280(5) 0.02716(15) Uani 1 1 d .
Mn2 Mn 0.0000 1.0000 0.0000 0.02651(19) Uani 1 2 d S
S1 S 0.17390(13) 0.28460(11) 0.52236(8) 0.0223(2) Uani 1 1 d .
S2 S 0.43244(14) 0.55905(12) 0.31807(9) 0.0268(2) Uani 1 1 d .
S3 S -0.01041(13) 0.43670(13) 0.23117(8) 0.0266(2) Uani 1 1 d .
S4 S 0.45385(14) 0.12864(13) 0.25410(9) 0.0307(2) Uani 1 1 d .
N1 N 0.2717(5) 0.8395(4) 0.5145(3) 0.0304(7) Uani 1 1 d .
H1A H 0.3678 0.8493 0.4518 0.046 Uiso 1 1 calc R
H1B H 0.3100 0.8713 0.5803 0.046 Uiso 1 1 calc R
H1C H 0.1540 0.9078 0.4915 0.046 Uiso 1 1 calc R
N2 N 0.2243(5) 0.7394(4) 0.0000(3) 0.0406(8) Uani 1 1 d .
H2A H 0.2841 0.7080 0.0717 0.061 Uiso 1 1 calc R
H2B H 0.3195 0.7509 -0.0630 0.061 Uiso 1 1 calc R
H2C H 0.1562 0.6584 -0.0086 0.061 Uiso 1 1 calc R
N3 N 0.0191(5) 0.9695(5) 0.2073(3) 0.0399(8) Uani 1 1 d .
H3A H 0.0757 0.8602 0.2375 0.060 Uiso 1 1 calc R
H3B H -0.1063 0.9953 0.2440 0.060 Uiso 1 1 calc R
H3C H 0.0955 1.0411 0.2222 0.060 Uiso 1 1 calc R
N4 N 0.2582(5) 1.1598(5) -0.0435(3) 0.0393(8) Uani 1 1 d .
H4A H 0.3036 1.1696 0.0276 0.059 Uiso 1 1 calc R
H4B H 0.2097 1.2652 -0.0853 0.059 Uiso 1 1 calc R
H4C H 0.3608 1.1061 -0.0894 0.059 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
S4 As1 S3 110.78(5) . .
S4 As1 S2 113.84(4) . .
S3 As1 S2 111.03(4) . .
S4 As1 S1 112.99(5) . .
S3 As1 S1 105.11(4) . .
S2 As1 S1 102.51(5) . .
N1 Mn1 S1 156.09(9) . .
N1 Mn1 S3 103.65(10) . 2_566
S1 Mn1 S3 95.25(4) . 2_566
N1 Mn1 S2 98.16(9) . 2_666
S1 Mn1 S2 95.95(4) . 2_666
S3 Mn1 S2 91.13(4) 2_566 2_666
N1 Mn1 S2 81.85(9) . .
S1 Mn1 S2 77.75(4) . .
S3 Mn1 S2 171.10(3) 2_566 .
S2 Mn1 S2 95.04(4) 2_666 .
N1 Mn1 S1 83.79(9) . 2_566
S1 Mn1 S1 85.83(4) . 2_566
S3 Mn1 S1 78.44(4) 2_566 2_566
S2 Mn1 S1 169.54(4) 2_666 2_566
S2 Mn1 S1 95.41(4) . 2_566
N3 Mn2 N3 180.000(1) 2_575 .
N3 Mn2 N2 90.25(13) 2_575 .
N3 Mn2 N2 89.75(14) . .
N3 Mn2 N2 89.75(14) 2_575 2_575
N3 Mn2 N2 90.25(14) . 2_575
N2 Mn2 N2 180.0 . 2_575
N3 Mn2 N4 92.19(13) 2_575 2_575
N3 Mn2 N4 87.81(13) . 2_575
N2 Mn2 N4 86.72(13) . 2_575
N2 Mn2 N4 93.28(13) 2_575 2_575
N3 Mn2 N4 87.81(13) 2_575 .
N3 Mn2 N4 92.19(13) . .
N2 Mn2 N4 93.28(13) . .
N2 Mn2 N4 86.72(13) 2_575 .
N4 Mn2 N4 180.000(1) 2_575 .
As1 S1 Mn1 92.37(4) . .
As1 S1 Mn1 83.47(4) . 2_566
Mn1 S1 Mn1 94.17(4) . 2_566
As1 S2 Mn1 107.17(4) . 2_666
As1 S2 Mn1 83.74(4) . .
Mn1 S2 Mn1 84.96(4) 2_666 .
As1 S3 Mn1 92.57(4) . 2_566
Mn1 N1 H1A 109.5 . .
Mn1 N1 H1B 109.5 . .
H1A N1 H1B 109.5 . .
Mn1 N1 H1C 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
Mn2 N2 H2A 109.5 . .
Mn2 N2 H2B 109.5 . .
H2A N2 H2B 109.5 . .
Mn2 N2 H2C 109.5 . .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
Mn2 N3 H3A 109.5 . .
Mn2 N3 H3B 109.5 . .
H3A N3 H3B 109.5 . .
Mn2 N3 H3C 109.5 . .
H3A N3 H3C 109.5 . .
H3B N3 H3C 109.5 . .
Mn2 N4 H4A 109.5 . .
Mn2 N4 H4B 109.5 . .
H4A N4 H4B 109.5 . .
Mn2 N4 H4C 109.5 . .
H4A N4 H4C 109.5 . .
H4B N4 H4C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
As1 S4 2.1283(12) .
As1 S3 2.1661(11) .
As1 S2 2.1825(11) .
As1 S1 2.1843(11) .
Mn1 N1 2.162(3) .
Mn1 S1 2.5356(11) .
Mn1 S3 2.5531(13) 2_566
Mn1 S2 2.6468(14) 2_666
Mn1 S2 2.8746(14) .
Mn1 S1 2.8936(14) 2_566
Mn2 N3 2.253(3) 2_575
Mn2 N3 2.253(3) .
Mn2 N2 2.297(3) .
Mn2 N2 2.297(3) 2_575
Mn2 N4 2.310(3) 2_575
Mn2 N4 2.310(3) .
S1 Mn1 2.8936(14) 2_566
S2 Mn1 2.6468(14) 2_666
S3 Mn1 2.5531(13) 2_566
N1 H1A 0.8900 .
N1 H1B 0.8900 .
N1 H1C 0.8900 .
N2 H2A 0.8900 .
N2 H2B 0.8900 .
N2 H2C 0.8900 .
N3 H3A 0.8900 .
N3 H3B 0.8900 .
N3 H3C 0.8900 .
N4 H4A 0.8900 .
N4 H4B 0.8900 .
N4 H4C 0.8900 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4C S4 0.89 2.86 3.685(4) 155.3 2_665
N4 H4B S3 0.89 2.77 3.647(4) 169.6 2_575
N4 H4A S4 0.89 2.72 3.596(4) 168.5 1_565
N3 H3C S4 0.89 2.71 3.531(4) 154.1 1_565
N3 H3B S4 0.89 2.91 3.739(4) 155.9 1_465
N2 H2C S3 0.89 3.01 3.676(4) 133.1 2_565
N2 H2B S4 0.89 2.59 3.458(4) 164.5 2_665
N2 H2A S2 0.89 2.92 3.803(4) 169.7 .
N1 H1C S1 0.89 2.96 3.420(3) 113.8 2_566
N1 H1B S4 0.89 2.54 3.372(3) 156.5 2_666
N1 H1A S2 0.89 2.91 3.343(3) 111.5 .
N1 H1A S4 0.89 2.89 3.574(3) 134.6 1_565
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
S4 As1 S1 Mn1 139.98(4) . .
S3 As1 S1 Mn1 -99.10(5) . .
S2 As1 S1 Mn1 17.04(4) . .
S4 As1 S1 Mn1 -126.09(4) . 2_566
S3 As1 S1 Mn1 -5.17(4) . 2_566
S2 As1 S1 Mn1 110.97(4) . 2_566
N1 Mn1 S1 As1 19.2(2) . .
S3 Mn1 S1 As1 161.58(3) 2_566 .
S2 Mn1 S1 As1 -106.73(4) 2_666 .
S2 Mn1 S1 As1 -12.84(3) . .
S1 Mn1 S1 As1 83.62(4) 2_566 .
N1 Mn1 S1 Mn1 -64.4(2) . 2_566
S3 Mn1 S1 Mn1 77.96(4) 2_566 2_566
S2 Mn1 S1 Mn1 169.65(4) 2_666 2_566
S2 Mn1 S1 Mn1 -96.47(4) . 2_566
S1 Mn1 S1 Mn1 0.0 2_566 2_566
S4 As1 S2 Mn1 -54.69(6) . 2_666
S3 As1 S2 Mn1 179.47(3) . 2_666
S1 As1 S2 Mn1 67.68(5) . 2_666
S4 As1 S2 Mn1 -137.43(4) . .
S3 As1 S2 Mn1 96.73(4) . .
S1 As1 S2 Mn1 -15.06(4) . .
N1 Mn1 S2 As1 -154.52(9) . .
S1 Mn1 S2 As1 12.92(3) . .
S3 Mn1 S2 As1 -25.7(2) 2_566 .
S2 Mn1 S2 As1 107.93(4) 2_666 .
S1 Mn1 S2 As1 -71.61(4) 2_566 .
N1 Mn1 S2 Mn1 97.55(9) . 2_666
S1 Mn1 S2 Mn1 -95.01(4) . 2_666
S3 Mn1 S2 Mn1 -133.7(2) 2_566 2_666
S2 Mn1 S2 Mn1 0.0 2_666 2_666
S1 Mn1 S2 Mn1 -179.54(3) 2_566 2_666
S4 As1 S3 Mn1 128.18(4) . 2_566
S2 As1 S3 Mn1 -104.29(5) . 2_566
S1 As1 S3 Mn1 5.83(4) . 2_566
