Insights from 125Te and 57Fe Nuclear Resonance Vibrational Spectroscopy: a [4Fe-4Te] Cluster from Two Points of View
Wittkamp, Florian; Mishra, Nakul; Wang, Hongxin; Wille, Hans-Christian; Steinbrügge, René; Kaupp, Martin; Cramer, Stephen P.; Apfel, Ulf-Peter; Pelmenschikov, Vladimir; Chemical Science  (2019) –; doi:10.1039/C9SC02025J

data_1551892
_publ_section_title
;
 Insights from 125Te and 57Fe Nuclear Resonance Vibrational Spectroscopy:
 a [4Fe-4Te] Cluster from Two Points of View
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02025J
_journal_year                    2019
_chemical_formula_moiety         'C24 H20 Fe4 S4 Te4, 3(C8 H20 N)'
_chemical_formula_sum            'C48 H80 Fe4 N3 S4 Te4'
_chemical_formula_weight         1561.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-04-08 deposited with the CCDC.    2019-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.0146(9)
_cell_length_b                   39.6995(13)
_cell_length_c                   12.1800(4)
_cell_measurement_reflns_used    22505
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      33.4830
_cell_measurement_theta_min      3.1940
_cell_volume                     12095.6(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 8.4171
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            74687
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         3.005
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.002
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       cube
_exptl_crystal_F_000             6120
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 2847 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.034(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         6945
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0216P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0548
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6390
_reflns_number_total             6945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02025j4.cif
_cod_data_source_block           (NEt4)3[Fe4Te4(SPh)4]
_cod_depositor_comments
;

2022-09-26
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         1248.95
_cod_original_formula_units_Z            10
_cod_original_formula_sum        'C38.40 H64 Fe3.20 N2.40 S3.20 Te3.20'
_cod_database_code               1551892
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              36223