Synthetic control over polymorph formation in the d-band semiconductor system FeS2
Ma, KeYuan; Lefèvre, Robin; Li, Qingtian; Lago, Jorge; Blacque, Olivier; Yang, Wanli; von Rohr, Fabian O.; Chemical Science  (2021) –; doi:10.1039/D1SC03026D

data_1564890
_publ_section_title
;
 Synthetic control over polymorph formation in the d-band semiconductor
 system FeS2
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC03026D
_journal_year                    2021
_chemical_formula_moiety         '0.25(Fe4 S8)'
_chemical_formula_sum            'Fe S2'
_chemical_formula_weight         119.97
_chemical_name_systematic        Pyrite
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_atom_sites_solution_primary     heavy
_audit_creation_date             2019-11-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-24 deposited with the CCDC.	2021-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.41027(15)
_cell_length_b                   5.41027(15)
_cell_length_c                   5.41027(15)
_cell_measurement_reflns_used    371
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      74.9570
_cell_measurement_theta_min      14.2510
_cell_volume                     158.364(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -130.00 -78.00   0.50    0.75    --  -54.56-109.00 175.00  104
  2  \w   -131.00 -35.00   0.50    0.75    --  -86.25 178.00-150.00  192
  3  \w     99.00 178.00   0.50    0.75    --  107.75  30.00 -30.00  158
  4  \w     37.00  71.00   0.50    0.75    --  107.75 -61.00 -60.00   68
  5  \w   -129.00 -75.00   0.50    0.75    --  -54.56 -87.00 -99.00  108
  6  \w   -131.00 -45.00   0.50    0.75    --  -54.56 -38.00  30.00  172
  7  \w     35.00 105.00   0.50    0.75    --  107.75 -77.00  60.00  140
  8  \w     37.00  62.00   0.50    0.75    --  107.75 -61.00-180.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.2047215000
_diffrn_orient_matrix_UB_12      -0.0480733000
_diffrn_orient_matrix_UB_13      -0.1919199000
_diffrn_orient_matrix_UB_21      0.1880919000
_diffrn_orient_matrix_UB_22      0.1329225000
_diffrn_orient_matrix_UB_23      0.1674201000
_diffrn_orient_matrix_UB_31      0.0616074000
_diffrn_orient_matrix_UB_32      -0.2472162000
_diffrn_orient_matrix_UB_33      0.1272811000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            509
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.914
_diffrn_reflns_theta_min         14.288
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    95.830
_exptl_absorpt_correction_T_max  0.290
_exptl_absorpt_correction_T_min  0.103
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.032
_exptl_crystal_description       irregular
_exptl_crystal_F_000             232
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.320
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7
_refine_ls_number_reflns         57
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.320
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0183
_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^)+(0.0160P)^2^+0.4779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0444
_reflns_Friedel_coverage         0.000
_reflns_number_gt                57
_reflns_number_total             57
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03026d2.cif
_cod_data_source_block           kema2910
_cod_original_cell_volume        158.364(13)
_cod_database_code               1564890
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.250
_shelx_estimated_absorpt_t_min   0.087
_olex2_refinement_description
;
;
_shelx_res_checksum              79445
_shelx_hkl_checksum              14296