Photoluminescent Re6Q8I2 (Q = S, Se) Semiconducting Cluster Compounds
Laing, Craig C.; Shen, Jiahong; Chica, Daniel G.; Cuthriell, Shelby A.; Schaller, Richard D.; Wolverton, Chris; Kanatzidis, Mercouri G.; Chemistry of Materials  (2021) –; doi:10.1021/acs.chemmater.1c01696

data_4004000
_publ_section_title
;
 Photoluminescent Re6Q8I2 (Q = S, Se) Semiconducting Cluster Compounds
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.1c01696
_journal_year                    2021
_chemical_formula_moiety         'Re6 S4 Se4 I2'
_chemical_formula_sum            'I2 Re6 S4 Se4'
_chemical_formula_weight         1815.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.20(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.4555(13)
_cell_length_b                   11.848(2)
_cell_length_c                   10.308(2)
_cell_measurement_reflns_used    8997
_cell_measurement_temperature    293
_cell_measurement_theta_max      31.54
_cell_measurement_theta_min      2.71
_cell_volume                     778.3(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Pilatus300K CdTe'
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  180
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56083
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8995
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        19.664
_diffrn_reflns_theta_max         26.495
_diffrn_reflns_theta_min         2.713
_diffrn_source                   'Axo Ag'
_diffrn_source_current           0.680
_diffrn_source_power             0.044
_diffrn_source_voltage           65
_exptl_absorpt_coefficient_mu    32.310
_exptl_absorpt_correction_T_max  0.0285
_exptl_absorpt_correction_T_min  0.0071
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    7.746
_exptl_crystal_description       needle
_exptl_crystal_F_000             1512
_exptl_crystal_preparation       'Grown in a NaI salt flux'
_exptl_crystal_recrystallization_method 'Grown in a NaI salt flux'
_exptl_crystal_size_max          0.011
_exptl_crystal_size_mid          0.006
_exptl_crystal_size_min          0.006
_refine_diff_density_max         3.393
_refine_diff_density_min         -2.918
_refine_diff_density_rms         0.678
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         3264
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+11.6236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2299
_reflns_number_total             3264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm1c01696_si_003.cif
_cod_data_source_block           try1
_cod_original_formula_sum        'Re6 S4 Se4 I2'
_cod_database_code               4004000
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.830
_shelx_estimated_absorpt_t_min   0.718
_olex2_refinement_description
;
1. Shared sites
{Se4, S4}
{Se2, S2}
{Se1, S1}
{Se3, S3}
2. Uiso/Uaniso restraints and constraints
Uanis(S4) = Uanis(Se4)
Uanis(Se4) = Uanis(S4)
Uanis(Se2) = Uanis(S2)
Uanis(S3) = Uanis(Se3)
Uanis(S1) = Uanis(Se1)
Uanis(Se1) = Uanis(S1)
Uanis(Se3) = Uanis(S3)
3. Others
 1*[Sof(S4)+Sof(Se4)]+1*[Sof(Se2)+Sof(S2)]+1*[Sof(S1)+Sof(Se1)]+1*[Sof(S3)+
 Sof(Se3)]=2 with esd of 0
 Sof(S4)=1-FVAR(1)
 Sof(Se4)=FVAR(1)
 Sof(S2)=1-FVAR(2)
 Sof(Se2)=FVAR(2)
 Sof(S1)=1-FVAR(3)
 Sof(Se1)=FVAR(3)
 Sof(S3)=1-FVAR(4)
 Sof(Se3)=FVAR(4)
;
_shelx_res_checksum              63414
_shelx_hkl_checksum              25018
_olex2_exptl_crystal_mounting_method 'super glued to a glass fiber'
_olex2_submission_special_instructions 'No special instructions were received'