Seleno-Analogous of Pentlandite (Fe4.5Ni4.5S8-ySey, Y = 1-6): Tuning bulk Fe/Ni Sulphoselenides for Hydrogen Evolution
Smialkowski, Mathias; Siegmund, Daniel; Pellumbi, Kevinjeorjios; Hensgen, Lars; Antoni, Hendrik; Muhler, Martin; Apfel, Ulf-Peter; Chemical Communications 55 (2019) 8792–8795; doi:10.1039/C9CC01842E

data_7123324
_publ_section_title
;
 Seleno-Analogous of Pentlandite (Fe4.5Ni4.5S8-ySey, Y = 1-6): Tuning bulk
 Fe/Ni Sulphoselenides for Hydrogen Evolution
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   60
_journal_name_full               'Chemical Communications'
_journal_page_first              8792
_journal_page_last               8795
_journal_paper_doi               10.1039/C9CC01842E
_journal_volume                  55
_journal_year                    2019
_chemical_formula_sum            'Fe18.63 Ni17.37 S28.1 Se3.9'
_chemical_formula_weight         3269.11
_chemical_name_common            Se1
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-02-07 deposited with the CCDC.    2019-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   10.1234(3)
_cell_length_b                   10.1234(3)
_cell_length_c                   10.1234(3)
_cell_measurement_reflns_used    319
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      30.0050
_cell_measurement_theta_min      4.0210
_cell_volume                     1037.48(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.782
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0097
_diffrn_reflns_av_unetI/netI     0.0088
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.782
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            398
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.782
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.091
_diffrn_reflns_theta_min         3.486
_exptl_absorpt_coefficient_mu    18.784
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.20a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    5.232
_exptl_crystal_description       plate
_exptl_crystal_F_000             1553
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     12
_refine_ls_number_reflns         86
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0105
_refine_ls_R_factor_gt           0.0104
_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^)+(0.0158P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0229
_refine_ls_wR_factor_ref         0.0229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                85
_reflns_number_total             86
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01842e2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
;
 Updated bibliographic information.

 Antanas Vaitkus,
 2021-04-22
;
_cod_original_cell_volume        1037.48(9)
_cod_original_formula_sum        'Fe18.63 Ni17.37 S28.10 Se3.90'
_cod_database_code               7123324
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.255
_shelx_estimated_absorpt_t_max   0.315
_shelx_res_checksum              81375