(NH4)4Sn2S6·3H2O: Crystal Structure, Thermal Decomposition, and Precursor for Textured Thin Film
Nørby, Peter; Overgaard, Jacob; Christensen, Per S.; Richter, Bo; Song, Xin; Dong, Mingdong; Han, Anpan; Skibsted, Jørgen; Iversen, Bo B.; Johnsen, Simon; Chemistry of Materials 26 (2014) 4494–; doi:10.1021/cm501681r

data_4002034
_publ_section_title
;
 (NH4)4Sn2S6&#x00B7;3H2O: Crystal Structure, Thermal Decomposition, and
 Precursor for Textured Thin Film
;
_journal_issue                   15
_journal_name_full               'Chemistry of Materials'
_journal_page_first              4494
_journal_paper_doi               10.1021/cm501681r
_journal_volume                  26
_journal_year                    2014
_chemical_formula_moiety         'S6 Sn2, 3(H2 O), 4(H4 N)'
_chemical_formula_sum            'H22 N4 O3 S6 Sn2'
_chemical_formula_weight         555.95
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-08-22
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.56294(8)
_cell_length_b                   8.56294(8)
_cell_length_c                   22.7703(3)
_cell_measurement_reflns_used    7389
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      29.2638
_cell_measurement_theta_min      2.3757
_cell_volume                     1669.61(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      99.97(11)
_diffrn_detector_area_resol_mean 10.3590
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.9877
_diffrn_measurement_details
;
  1 omega  -13.00   79.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5301   77.0000 -150.0000 92

  2 omega    3.00   83.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5301   57.0000   90.0000 80

  3 omega  -38.00   -1.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.7801   38.0000 -180.0000 37

  4 omega -102.00  -35.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.7801 -178.0000  -60.0000 67
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0116849000
_diffrn_orient_matrix_UB_12      0.0269702000
_diffrn_orient_matrix_UB_13      0.0291378000
_diffrn_orient_matrix_UB_21      -0.0487787000
_diffrn_orient_matrix_UB_22      -0.0606912000
_diffrn_orient_matrix_UB_23      0.0107307000
_diffrn_orient_matrix_UB_31      0.0660269000
_diffrn_orient_matrix_UB_32      -0.0495880000
_diffrn_orient_matrix_UB_33      0.0027623000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            21147
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.630
_diffrn_reflns_theta_min         2.541
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.738
_exptl_absorpt_correction_T_max  0.468
_exptl_absorpt_correction_T_min  0.359
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            'clear yellowish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.212
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.0853
_exptl_crystal_size_mid          0.0706
_exptl_crystal_size_min          0.0549
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 1577 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.011(9)
_refine_ls_extinction_coef       0.00162(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         4315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0185
_refine_ls_R_factor_gt           0.0162
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0092P)^2^+0.5443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0313
_refine_ls_wR_factor_ref         0.0322
_reflns_Friedel_coverage         0.670
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                4109
_reflns_number_total             4315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm501681r_si_002.cif
_cod_data_source_block           nh4sns_x
_cod_depositor_comments          'Adding full bibliography for 4002034.cif.'
_cod_original_cell_volume        1669.61(4)
_cod_database_code               4002034
_chemical_oxdiff_formula         'H22 N4 S6 Sn2 O3 '
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_shelxl_version_number           2013-4