Visualization of a Discrete Solid-State Process with Steady-State X-ray Diffraction: Observation of Hopping of Sulfur Atoms in Single Crystals of Realgar
Panče Naumov; Petre Makreski; Gjorgji Petruševski; Tomče Runčevski; Gligor Jovanovski; Journal of the American Chemical Society 132 (2010) 11398–11401; doi:10.1021/ja1030672

data_4102899
_publ_section_title
;
 Visualization of a Discrete Solid-State Process with Steady-State X-ray
 Diffraction: Observation of Hopping of Sulfur Atoms in Single Crystals of
 Realgar
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11398
_journal_page_last               11401
_journal_paper_doi               10.1021/ja1030672
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'As4 S4'
_chemical_formula_weight         427.92
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/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                 106.178(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3316(11)
_cell_length_b                   13.5678(16)
_cell_length_c                   6.5866(7)
_cell_measurement_temperature    293(2)
_cell_volume                     800.90(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.856
_diffrn_measured_fraction_theta_max 0.856
_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  0.0954
_diffrn_reflns_av_sigmaI/netI    0.1295
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11006
_diffrn_reflns_theta_full        38.39
_diffrn_reflns_theta_max         38.39
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    17.484
_exptl_crystal_density_diffrn    3.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             784
_refine_diff_density_max         2.246
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.365
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.894
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         3838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.894
_refine_ls_R_factor_all          0.1942
_refine_ls_R_factor_gt           0.0828
_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
 [0.00000+1.00000exp(3.00(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0400+0.0000*P+(0.1086P)^2^+0.0000sin\q/\l]
 where P = 0.10000Fo^2^ + 0.90000Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2118
_refine_ls_wR_factor_ref         0.2882
_reflns_number_gt                1735
_reflns_number_total             3838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1030672_re11-12.cif
_cod_data_source_block           re11-12
_cod_database_code               4102899