pH-induced solvothermal synthesis and characterization of two novel thioarsenate compounds: Three-dimensional (1,2-pdaH2)0.5As5S8 containing ψ-As(iii)S4 and two-dimensional (NH4)2As8S13
Du, Ke-Zhao; Feng, Mei-Ling; Li, Jian-Rong; Huang, Xiao-Ying; CrystEngComm 14 (2012) 4959–; doi:10.1039/c2ce25475a

data_7208332
_publ_section_title
;
 pH-induced solvothermal synthesis and characterization of two novel
 thioarsenate compounds: Three-dimensional (1,2-pdaH2)0.5As5S8 containing
 \y-As(iii)S4 and two-dimensional (NH4)2As8S13
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              4959
_journal_paper_doi               10.1039/c2ce25475a
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'As5 S8, C1.5 N H6'
_chemical_formula_sum            'C1.5 H6 As5 N S8'
_chemical_formula_weight         669.15
_chemical_name_systematic
;
?
;
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   14.070(4)
_cell_length_b                   15.300(4)
_cell_length_c                   27.431(8)
_cell_measurement_reflns_used    4292
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.5087
_cell_measurement_theta_min      2.1008
_cell_volume                     5905(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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      123
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            10480
_diffrn_reflns_theta_full        26.75
_diffrn_reflns_theta_max         26.75
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    12.300
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    3.011
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             5040
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.1410
_exptl_crystal_size_min          0.1240
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1576
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0205
_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/[\s^2^(Fo^2^)+(0.0280P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0497
_reflns_number_gt                1443
_reflns_number_total             1576
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25475a.txt
_cod_data_source_block           compound-1-kd4-26c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'F d d d'
_cod_original_formula_sum        'C1.50 H6 As5 N S8'
_cod_database_code               7208332