#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:46:55 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178963 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/92/4119241.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_4119241
loop_
_publ_author_name
'Wei-Wei Xiong'
'Eashwer Umesh Athresh'
'Yu Ting Ng'
'Junfeng Ding'
'Tom Wu'
'Qichun Zhang'
_publ_section_title
;
 Growing Crystalline Chalcogenidoarsenates in Surfactants: From
 Zero-Dimensional Cluster to Three-Dimensional Framework
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1256
_journal_page_last               1259
_journal_paper_doi               10.1021/ja3116179
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         '2(As H4 Mn N2 S4), H18 Mn N6'
_chemical_formula_sum            'As2 H26 Mn3 N10 S8'
_chemical_formula_weight         737.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.21(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.312(5)
_cell_length_b                   7.9301(16)
_cell_length_c                   12.412(3)
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.14
_cell_volume                     2389.2(9)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'DIAMOND. Version 3.0. Crystal Impact'
_computing_publication_material  'Windows Word 2003'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11072
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    5.017
_exptl_absorpt_correction_T_max  0.4368
_exptl_absorpt_correction_T_min  0.3966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.050
_exptl_crystal_description       plate
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         2715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0247
_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)+(0.0200P)²+15.5413P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                2458
_reflns_number_total             2715
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3116179_si_003.cif
_cod_data_source_block           y2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4119241
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Mn1 Mn 0.245025(19) 0.02097(6) 0.48828(4) 0.02184(11) Uani 1 1 d .
Mn2 Mn 0.0000 0.76172(9) 0.2500 0.02633(15) Uani 1 2 d S
As1 As 0.142604(12) 0.27802(4) 0.41955(2) 0.01888(8) Uani 1 1 d .
S1 S 0.05524(3) 0.28460(12) 0.41753(7) 0.03301(19) Uani 1 1 d .
S2 S 0.17073(3) 0.06314(10) 0.33051(6) 0.02545(16) Uani 1 1 d .
S3 S 0.18401(3) 0.25094(9) 0.57989(6) 0.02130(15) Uani 1 1 d .
S4 S 0.17709(3) 0.51071(10) 0.35967(6) 0.02482(16) Uani 1 1 d .
N1 N 0.19444(11) -0.1804(3) 0.5716(2) 0.0257(5) Uani 1 1 d .
H1A H 0.1737 -0.1171 0.6203 0.031 Uiso 1 1 d R
H1B H 0.1742 -0.2275 0.5259 0.031 Uiso 1 1 d R
N2 N 0.27521(11) -0.1800(3) 0.3774(2) 0.0260(5) Uani 1 1 d .
H2A H 0.2961 -0.1259 0.3271 0.031 Uiso 1 1 d R
H2B H 0.2477 -0.2440 0.3241 0.031 Uiso 1 1 d R
N3 N 0.04968(14) 0.9666(4) 0.1700(3) 0.0448(8) Uani 1 1 d .
H3A H 0.0742 0.9283 0.1297 0.054 Uiso 1 1 d R
H3B H 0.0675 1.0350 0.2233 0.054 Uiso 1 1 d R
H3C H 0.0267 1.0394 0.1332 0.054 Uiso 1 1 d R
N4 N -0.05818(13) 0.7694(4) 0.0993(3) 0.0401(7) Uani 1 1 d .
H4A H -0.0436 0.7185 0.0466 0.048 Uiso 1 1 d R
H4B H -0.0514 0.8680 0.0667 0.048 Uiso 1 1 d R
H4C H -0.0890 0.7203 0.1109 0.048 Uiso 1 1 d R
N5 N 0.05420(12) 0.5592(4) 0.1821(2) 0.0350(6) Uani 1 1 d .
H5A H 0.0458 0.5457 0.1135 0.042 Uiso 1 1 d R
H5B H 0.0493 0.4642 0.2155 0.042 Uiso 1 1 d R
H5C H 0.0888 0.5882 0.1908 0.042 Uiso 1 1 d R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
As As 0.0499 2.0058 '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'
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
N2 Mn1 N1 89.09(10) . .
N2 Mn1 S4 97.21(7) . 7_556
N1 Mn1 S4 89.59(7) . 7_556
N2 Mn1 S2 82.41(7) . .
N1 Mn1 S2 93.51(7) . .
S4 Mn1 S2 176.87(3) 7_556 .
N2 Mn1 S3 163.39(8) . .
N1 Mn1 S3 87.62(7) . .
S4 Mn1 S3 99.04(3) 7_556 .
S2 Mn1 S3 81.55(3) . .
N2 Mn1 S3 92.71(7) . 7_556
N1 Mn1 S3 170.29(7) . 7_556
S4 Mn1 S3 80.72(3) 7_556 7_556
S2 Mn1 S3 96.19(3) . 7_556
S3 Mn1 S3 93.27(3) . 7_556
N5 Mn2 N5 89.91(16) 2 .
N5 Mn2 N4 88.69(11) 2 .
N5 Mn2 N4 93.48(12) . .
N5 Mn2 N4 93.48(12) 2 2
N5 Mn2 N4 88.69(11) . 2
N4 Mn2 N4 176.94(17) . 2
N5 Mn2 N3 90.57(12) 2 2
N5 Mn2 N3 175.43(11) . 2
N4 Mn2 N3 91.07(12) . 2
N4 Mn2 N3 86.75(12) 2 2
N5 Mn2 N3 175.43(11) 2 .
N5 Mn2 N3 90.57(12) . .
N4 Mn2 N3 86.75(12) . .
N4 Mn2 N3 91.07(12) 2 .
N3 Mn2 N3 89.32(19) 2 .
S1 As1 S2 110.98(4) . .
S1 As1 S4 112.31(4) . .
S2 As1 S4 110.79(4) . .
S1 As1 S3 114.94(4) . .
S2 As1 S3 104.16(3) . .
S4 As1 S3 103.15(3) . .
As1 S2 Mn1 86.73(3) . .
As1 S3 Mn1 85.26(3) . .
As1 S3 Mn1 85.29(3) . 7_556
Mn1 S3 Mn1 86.73(3) . 7_556
As1 S4 Mn1 87.09(3) . 7_556
N2 N1 Mn1 116.96(18) 7_546 .
N2 N1 H1A 113.4 7_546 .
Mn1 N1 H1A 103.6 . .
N2 N1 H1B 103.0 7_546 .
Mn1 N1 H1B 108.7 . .
H1A N1 H1B 111.2 . .
N1 N2 Mn1 116.52(18) 7_546 .
N1 N2 H2A 111.1 7_546 .
Mn1 N2 H2A 107.0 . .
N1 N2 H2B 101.3 7_546 .
Mn1 N2 H2B 120.7 . .
H2A N2 H2B 98.8 . .
Mn2 N3 H3A 113.8 . .
Mn2 N3 H3B 109.8 . .
H3A N3 H3B 107.9 . .
Mn2 N3 H3C 110.3 . .
H3A N3 H3C 111.0 . .
H3B N3 H3C 103.5 . .
Mn2 N4 H4A 110.3 . .
Mn2 N4 H4B 105.7 . .
H4A N4 H4B 88.4 . .
Mn2 N4 H4C 110.8 . .
H4A N4 H4C 108.3 . .
H4B N4 H4C 130.5 . .
Mn2 N5 H5A 109.9 . .
Mn2 N5 H5B 109.7 . .
H5A N5 H5B 109.1 . .
Mn2 N5 H5C 110.1 . .
H5A N5 H5C 109.0 . .
H5B N5 H5C 109.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 N2 2.255(3) .
Mn1 N1 2.296(3) .
Mn1 S4 2.6096(12) 7_556
Mn1 S2 2.6102(12) .
Mn1 S3 2.6473(10) .
Mn1 S3 2.6699(10) 7_556
Mn2 N5 2.269(3) 2
Mn2 N5 2.269(3) .
Mn2 N4 2.282(3) .
Mn2 N4 2.282(3) 2
Mn2 N3 2.284(3) 2
Mn2 N3 2.284(3) .
As1 S1 2.1234(9) .
As1 S2 2.1627(9) .
As1 S4 2.1748(9) .
As1 S3 2.1899(10) .
S3 Mn1 2.6699(10) 7_556
S4 Mn1 2.6096(12) 7_556
N1 N2 1.456(4) 7_546
N1 H1A 0.9517 .
N1 H1B 0.8200 .
N2 N1 1.456(4) 7_546
N2 H2A 0.9307 .
N2 H2B 1.0455 .
N3 H3A 0.8548 .
N3 H3B 0.9421 .
N3 H3C 0.9080 .
N4 H4A 0.8621 .
N4 H4B 0.8999 .
N4 H4C 0.8641 .
N5 H5A 0.8712 .
N5 H5B 0.8712 .
N5 H5C 0.8726 .
