{Ge8[Fe(CO)4]8}7−: An Anionic Cubic Germanium-Iron-Cluster Featuring an Unpaired Electron.
Schnepf, Andreas; Schrenk, Claudio; Preißing, Lars; Dalton Transactions  (2022) –; doi:10.1039/D2DT01090A

data_7710269
_publ_section_title
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 {Ge8[Fe(CO)4]8}7&#x2212;: An Anionic Cubic Germanium-Iron-Cluster
 Featuring an Unpaired Electron.
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01090A
_journal_year                    2022
_chemical_formula_moiety         'C88 H112 Fe8 Ge8 Na6 O46, C24 H48 Na O6'
_chemical_formula_sum            'C112 H160 Fe8 Ge8 Na7 O52'
_chemical_formula_weight         3526.84
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_Hall           '-I 2 2'
_space_group_name_H-M_alt        'I m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-18
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-04-07 deposited with the CCDC.	2022-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.6543(17)
_cell_length_b                   19.469(3)
_cell_length_c                   23.229(3)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.206
_cell_measurement_theta_min      2.420
_cell_volume                     7079.6(16)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.01
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            73698
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.427
_diffrn_reflns_theta_min         2.092
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.566
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1198 before and 0.0505 after correction.
The Ratio of minimum to maximum transmission is 0.8123.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_description       block
_exptl_crystal_F_000             3578
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: thf, toluene'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.073
_refine_diff_density_max         1.273
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         3983
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0603P)^2^+106.1188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3402
_reflns_number_total             3983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01090a2.cif
_cod_data_source_block           68
_cod_original_cell_volume        7079.7(15)
_cod_database_code               7710269
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.427
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 O301-C303 = O301-C304
 2.34 with sigma of 0.04
 C103-C102
 1.54 with sigma of 0.02
 C103-C103_$1
 1.54 with sigma of 0.02
 C302-C303 = C303-C304 = C304-C305
 1.54 with sigma of 0.02
 C302-C304 = C302-C305 = C303-C305
 2.34 with sigma of 0.04
 H30J-H30J_$3
 0.4 with sigma of 0.02
 O301-C302 \\sim O301-C305
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C15) \\sim Ueq, Uanis(C15A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O201) \\sim Ueq, Uanis(C205) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C102) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C308) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O301, C302, C303, C304, C305
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O14(0.5) O16(0.5) O16A(0.5) O24(0.5) O26(0.5) O26A(0.5) C13(0.5)
 C15(0.5) C15A(0.5) C23(0.5) C25(0.5) C25A(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
 H10D(0.5) C302(0.5) H30A(0.5) H30B(0.5) C303(0.5) H30C(0.5) H30D(0.5)
 H30E(0.5) H30F(0.5) H30G(0.5) H30H(0.5) C307(0.5) H30I(0.5) H30J(0.5)
 C308(0.5) H30K(0.5) H30L(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C102(H10A,H10B), C103(H10C,H10D), C202(H20A,H20B), C203(H20C,H20D), C204(H20E,
 H20F), C205(H20G,H20H), C207(H20I,H20J), C208(H20K,H20L), C302(H30A,H30B),
 C303(H30C,H30D), C304(H30E,H30F), C305(H30G,H30H), C307(H30I,H30J), C308(H30K,
 H30L)
;
_shelx_res_checksum              3201
_olex2_submission_special_instructions 'No special instructions were received'