#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:46:55 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178963 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/92/4119240.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_4119240
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         'As4 Mn2 S16, 8(H4 N)'
_chemical_formula_sum            'As4 H32 Mn2 N8 S16'
_chemical_formula_weight         1067.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 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                 96.047(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.2086(4)
_cell_length_b                   8.8211(4)
_cell_length_c                   20.7793(10)
_cell_measurement_reflns_used    6649
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      28.96
_cell_measurement_theta_min      2.34
_cell_volume                     1678.51(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'DIAMOND. Version 3.0. Crystal Impact'
_computing_publication_material  'Windows Word 2003'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            18598
_diffrn_reflns_theta_full        29.11
_diffrn_reflns_theta_max         29.11
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    5.673
_exptl_absorpt_correction_T_max  0.5493
_exptl_absorpt_correction_T_min  0.3966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.111
_exptl_crystal_description       block
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         4472
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0118P)²+0.6214P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0427
_refine_ls_wR_factor_ref         0.0440
_reflns_number_gt                3964
_reflns_number_total             4472
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3116179_si_002.cif
_cod_data_source_block           chen15
_cod_database_code               4119240
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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
As1 As 0.00216(2) 1.16152(2) 0.609725(9) 0.00766(5) Uani 1 1 d .
As2 As 0.44440(2) 0.69823(2) 0.625614(9) 0.00805(5) Uani 1 1 d .
Mn1 Mn 0.16908(3) 0.87532(4) 0.540456(14) 0.00928(7) Uani 1 1 d .
N1 N 0.2500 0.4070(3) 0.7500 0.0147(5) Uani 1 2 d SD
H1 H 0.1686(19) 0.347(2) 0.7421(12) 0.022 Uiso 1 1 d D
H2 H 0.255(3) 0.469(2) 0.7158(8) 0.022 Uiso 1 1 d D
N2 N 0.6267(2) 0.5971(3) 0.83458(11) 0.0344(6) Uani 1 1 d D
H3 H 0.614(3) 0.645(3) 0.7966(8) 0.052 Uiso 1 1 d D
H4 H 0.7245(14) 0.585(3) 0.8462(12) 0.052 Uiso 1 1 d D
H5 H 0.588(3) 0.652(3) 0.8647(10) 0.052 Uiso 1 1 d D
H6 H 0.588(3) 0.5046(17) 0.8315(12) 0.052 Uiso 1 1 d D
N3 N 0.2500 0.9398(3) 0.7500 0.0146(5) Uani 1 2 d SD
H7 H 0.236(2) 1.001(2) 0.7153(8) 0.022 Uiso 1 1 d D
H8 H 0.1694(19) 0.880(2) 0.7526(11) 0.022 Uiso 1 1 d D
N4 N 0.60791(19) 0.1223(2) 0.63869(9) 0.0150(4) Uani 1 1 d D
H9 H 0.6942(16) 0.164(2) 0.6566(9) 0.023 Uiso 1 1 d D
H10 H 0.588(2) 0.0410(18) 0.6642(8) 0.023 Uiso 1 1 d D
H11 H 0.5360(17) 0.1917(19) 0.6391(10) 0.023 Uiso 1 1 d D
H12 H 0.617(2) 0.089(2) 0.5981(6) 0.023 Uiso 1 1 d D
N5 N 0.2858(2) 0.3840(2) 0.50683(9) 0.0138(4) Uani 1 1 d D
H13 H 0.338(2) 0.407(3) 0.5443(8) 0.021 Uiso 1 1 d D
H14 H 0.1926(15) 0.379(3) 0.5124(11) 0.021 Uiso 1 1 d D
H15 H 0.297(3) 0.454(2) 0.4767(9) 0.021 Uiso 1 1 d D
H16 H 0.322(2) 0.2950(19) 0.4939(11) 0.021 Uiso 1 1 d D
S1 S -0.05704(6) 1.22217(7) 0.70338(2) 0.01469(11) Uani 1 1 d .
S2 S -0.06311(5) 1.33336(6) 0.53840(2) 0.01086(10) Uani 1 1 d .
S3 S -0.10592(5) 0.95662(6) 0.56907(2) 0.00966(10) Uani 1 1 d .
S4 S 0.23294(5) 1.11468(6) 0.61068(2) 0.00960(10) Uani 1 1 d .
S5 S 0.21230(5) 0.67031(6) 0.63268(2) 0.01153(10) Uani 1 1 d .
S6 S 0.45150(5) 0.83860(6) 0.53994(2) 0.01011(10) Uani 1 1 d .
S7 S 0.54532(6) 0.47979(6) 0.61703(3) 0.01530(11) Uani 1 1 d .
S8 S 0.55860(6) 0.80713(6) 0.70851(2) 0.01444(11) Uani 1 1 d .
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'
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'
H H 0.0000 0.0000 '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
S1 As1 S2 111.64(2) . .
S1 As1 S4 112.52(2) . .
S2 As1 S4 110.02(2) . .
S1 As1 S3 114.05(2) . .
S2 As1 S3 103.43(2) . .
S4 As1 S3 104.60(2) . .
S8 As2 S7 106.70(2) . .
S8 As2 S5 113.49(2) . .
S7 As2 S5 109.90(2) . .
S8 As2 S6 110.32(2) . .
S7 As2 S6 113.01(2) . .
S5 As2 S6 103.57(2) . .
S2 Mn1 S4 169.14(2) 3_576 .
S2 Mn1 S6 102.575(19) 3_576 .
S4 Mn1 S6 86.374(18) . .
S2 Mn1 S5 89.444(19) 3_576 .
S4 Mn1 S5 98.125(19) . .
S6 Mn1 S5 81.040(17) . .
S2 Mn1 S3 79.928(17) 3_576 3_576
S4 Mn1 S3 92.448(18) . 3_576
S6 Mn1 S3 100.847(18) . 3_576
S5 Mn1 S3 169.37(2) . 3_576
S2 Mn1 S3 91.603(18) 3_576 .
S4 Mn1 S3 79.988(17) . .
S6 Mn1 S3 165.29(2) . .
S5 Mn1 S3 95.364(18) . .
S3 Mn1 S3 85.331(17) 3_576 .
H1 N1 H2 109(2) . .
H3 N2 H4 108.9(15) . .
H3 N2 H5 109.9(15) . .
H4 N2 H5 109.4(15) . .
H3 N2 H6 110.9(15) . .
H4 N2 H6 106.9(15) . .
H5 N2 H6 110.8(16) . .
H7 N3 H8 110(2) . .
H9 N4 H10 107.3(13) . .
H9 N4 H11 109.2(14) . .
H10 N4 H11 109.2(13) . .
H9 N4 H12 110.4(14) . .
H10 N4 H12 109.0(14) . .
H11 N4 H12 111.6(13) . .
H13 N5 H14 110(2) . .
H13 N5 H15 111(2) . .
H14 N5 H15 108(2) . .
H13 N5 H16 106(2) . .
H14 N5 H16 114(2) . .
H15 N5 H16 109(2) . .
As1 S2 Mn1 89.68(2) . 3_576
As1 S3 Mn1 85.500(18) . 3_576
As1 S3 Mn1 84.688(18) . .
Mn1 S3 Mn1 94.669(17) 3_576 .
As1 S4 Mn1 89.198(19) . .
As2 S5 Mn1 86.980(19) . .
As2 S6 Mn1 87.226(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
As1 S1 2.1433(5) .
As1 S2 2.1606(5) .
As1 S4 2.1630(5) .
As1 S3 2.1894(5) .
As2 S8 2.1480(6) .
As2 S7 2.1548(6) .
As2 S5 2.1717(5) .
As2 S6 2.1751(5) .
Mn1 S2 2.5863(6) 3_576
Mn1 S4 2.5986(6) .
Mn1 S6 2.6220(6) .
Mn1 S5 2.6345(6) .
Mn1 S3 2.7272(6) 3_576
Mn1 S3 2.7565(6) .
N1 H1 0.918(13) .
N1 H2 0.902(13) .
N2 H3 0.893(13) .
N2 H4 0.913(13) .
N2 H5 0.893(13) .
N2 H6 0.891(13) .
N3 H7 0.900(13) .
N3 H8 0.915(13) .
N4 H9 0.918(12) .
N4 H10 0.922(12) .
N4 H11 0.903(12) .
N4 H12 0.905(12) .
N5 H13 0.895(13) .
N5 H14 0.878(13) .
N5 H15 0.896(13) .
N5 H16 0.906(13) .
S2 Mn1 2.5863(6) 3_576
S3 Mn1 2.7272(6) 3_576
