Phase Separation and Suppression of the Structural and Magnetic Transitions in Superconducting Doped Iron Tellurides, Fe1+xTe1-ySy
Pawel Zajdel; Ping-Yen Hsieh; Efrain E. Rodriguez; Nicholas P. Butch; Jeff D. Magill; Johnpierre Paglione; Peter Zavalij; Matthew R. Suchomel; Mark A. Green; Journal of the American Chemical Society 132 (2010) 13000–13007; doi:10.1021/ja105279p

data_4103059
_publ_section_title
;
 Phase Separation and Suppression of the Structural and Magnetic
 Transitions in Superconducting Doped Iron Tellurides, Fe1+xTe1-ySy
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13000
_journal_page_last               13007
_journal_paper_doi               10.1021/ja105279p
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'Fe1.13 S0.05 Te0.95'
_chemical_formula_sum            'Fe1.13 S0.05 Te0.95'
_chemical_formula_weight         185.25
_chemical_name_common            'Iron telluride'
_chemical_name_systematic
;
Iron telluride
;
_space_group_IT_number           129
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2a'
_symmetry_space_group_name_H-M   'P 4/n m m :2'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   3.81590(10)
_cell_length_b                   3.81590(10)
_cell_length_c                   6.2460(3)
_cell_measurement_reflns_used    2737
_cell_measurement_temperature    249(2)
_cell_measurement_theta_max      52.2
_cell_measurement_theta_min      3.3
_cell_volume                     90.949(6)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      249(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 11.198
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      370,370,370,370,370,370,200
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0046278
_diffrn_orient_matrix_UB_12      0.0191914
_diffrn_orient_matrix_UB_13      -0.1596346
_diffrn_orient_matrix_UB_21      0.1918737
_diffrn_orient_matrix_UB_22      -0.1776669
_diffrn_orient_matrix_UB_23      -0.0100797
_diffrn_orient_matrix_UB_31      -0.1783925
_diffrn_orient_matrix_UB_32      -0.1917526
_diffrn_orient_matrix_UB_33      -0.0067027
_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  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0160
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1870
_diffrn_reflns_theta_full        44.84
_diffrn_reflns_theta_max         44.84
_diffrn_reflns_theta_min         6.27
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    23.650
_exptl_absorpt_correction_T_max  0.701
_exptl_absorpt_correction_T_min  0.019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP (Sheldrick, 1997)'
_exptl_crystal_colour            silver
_exptl_crystal_density_diffrn    6.779
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       plate
_exptl_crystal_F_000             159
_exptl_crystal_id                'NIST/Ping-Yen Fe1.15Te0.95S0.05'
_exptl_crystal_size_max          0.405
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.015
_refine_diff_density_max         2.947
_refine_diff_density_min         -1.257
_refine_diff_density_rms         0.306
_refine_ls_extinction_coef       0.008(2)
_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   1.000
_refine_ls_matrix_type           full
_refine_ls_number_parameters     13
_refine_ls_number_reflns         250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0193
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.01P)^2^+0.8035P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0422
_refine_ls_wR_factor_ref         0.0423
_reflns_number_gt                249
_reflns_number_total             250
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja105279p_si_002.cif
_cod_data_source_block           1715
_cod_original_sg_symbol_H-M      'P 4/n m m'
_cod_database_code               4103059
_diffrn_measurement_frame_width-ccd -0.5
_diffrn_measurement_total_frames-ccd 2420
_diffrn_measurement_frame_time-ccd 15
_diffrn_measurement_total_time-ccd 14.1
_diffrn_detector_distance-ccd    5.2000
_diffrn_measurement_frame_size-ccd 512