# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

 
data_Ge12I8{Fe(CO)3}8
 
_publ_contact_author_name        'Claus Feldmann'
_publ_contact_author_address     
'Inst. fuer Anorg. Chemie, KIT, Engesserstr. 15, D-76131 Karlsruhe, Germany'
_publ_contact_author_email       claus.feldmann@kit.edu
_publ_contact_author_phone       +49-721-608-42855
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C24 Fe8 Ge12 I4 O24' 
_chemical_formula_weight          2497.72

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe'  'Fe'   0.3463   0.8444
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ge'  'Ge'   0.1547   1.8001
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'I'  'I'  -0.4742   1.8119
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/n'
_space_group_name_Hall            '-P 2yn'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    11.8483(4)
_cell_length_b                    18.5480(7)
_cell_length_c                    12.1901(4)
_cell_angle_alpha                 90
_cell_angle_beta                  110.483(3)
_cell_angle_gamma                 90
_cell_volume                      2509.55(16)
_cell_formula_units_Z             2
_cell_measurement_temperature     200(2)
_cell_measurement_reflns_used     25416 
_cell_measurement_theta_min       2.29 
_cell_measurement_theta_max       59.53 
 
_exptl_crystal_description        prism 
_exptl_crystal_colour             red 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured'               
_exptl_crystal_density_diffrn     3.305          
_exptl_crystal_F_000              2280
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.502 
_exptl_crystal_size_mid           0.471 
_exptl_crystal_size_min           0.436
_exptl_absorpt_coefficient_mu     11.831
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    numerical 
_exptl_absorpt_correction_T_min   0.2022 
_exptl_absorpt_correction_T_max   0.3970
_exptl_absorpt_process_details    '(X-RED, Data Reduction Program, Version 1.14, Stoe & Cie GmbH, Darmstadt 1999.; X-SHAPE, Crystal Optimisation for Numerical Absorption Correction, Version 1.06, Stoe & Cie GmbH, Darmstadt 1999.)' 
  
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       200(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine-focus sealed tube'  
_diffrn_radiation_monochromator   graphite                      
_diffrn_measurement_device_type   'STOE IPDS II'  
_diffrn_measurement_method        'image plate'  
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             25060
_diffrn_reflns_av_unetI/netI      0.0771
_diffrn_reflns_av_R_equivalents   0.1190
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -25
_diffrn_reflns_limit_k_max        25
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          2.063
_diffrn_reflns_theta_max          29.648
_diffrn_reflns_theta_full         26.000
_diffrn_measured_fraction_theta_max   0.956
_diffrn_measured_fraction_theta_full  0.977
_diffrn_reflns_Laue_measured_fraction_max    0.956
_diffrn_reflns_Laue_measured_fraction_full   0.977
_diffrn_reflns_point_group_measured_fraction_max   0.956
_diffrn_reflns_point_group_measured_fraction_full  0.977
_reflns_number_total              6774
_reflns_number_gt                 4459
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0159P)²+20.0658P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          6774
_refine_ls_number_parameters      325
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0943
_refine_ls_R_factor_gt            0.0473
_refine_ls_wR_factor_ref          0.0936
_refine_ls_wR_factor_gt           0.0791
_refine_ls_goodness_of_fit_ref    1.058
_refine_ls_restrained_S_all       1.058
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
I1 I 0.91887(5) 0.41969(3) 0.57123(5) 0.02925(13) Uani 1 1 d . . . . .
I2 I 0.54662(6) 0.69920(3) 0.21881(5) 0.02842(13) Uani 1 1 d . . . . .
Ge1 Ge 0.65462(8) 0.52924(5) 0.61846(7) 0.02052(18) Uani 1 1 d . . . . .
Ge2 Ge 0.56478(8) 0.42943(5) 0.41705(7) 0.02109(18) Uani 1 1 d . . . . .
Ge3 Ge 0.49179(8) 0.55996(5) 0.26967(7) 0.02093(18) Uani 1 1 d . . . . .
Ge4 Ge 0.56557(8) 0.64343(5) 0.44334(8) 0.02142(18) Uani 1 1 d . . . . .
Ge5 Ge 0.75716(8) 0.51793(5) 0.45296(8) 0.02311(18) Uani 1 1 d . . . . .
Ge6 Ge 0.30590(9) 0.61788(5) 0.35689(8) 0.0274(2) Uani 1 1 d . . . . .
Fe1 Fe 0.77041(11) 0.62340(6) 0.56291(10) 0.0211(2) Uani 1 1 d . . . . .
C1 C 0.8252(9) 0.6782(5) 0.4708(8) 0.032(2) Uani 1 1 d . . . . .
O1 O 0.8615(7) 0.7138(4) 0.4141(6) 0.0435(18) Uani 1 1 d . . . . .
C2 C 0.9145(9) 0.5969(4) 0.6658(8) 0.0293(19) Uani 1 1 d . . . . .
O2 O 1.0059(6) 0.5829(4) 0.7332(6) 0.0467(18) Uani 1 1 d . . . . .
C3 C 0.7500(8) 0.6935(5) 0.6522(8) 0.0291(19) Uani 1 1 d . . . . .
O3 O 0.7385(7) 0.7423(4) 0.7057(6) 0.0466(19) Uani 1 1 d . . . . .
Fe2 Fe 0.27481(11) 0.54183(6) 0.19988(10) 0.0212(2) Uani 1 1 d . . . . .
C4 C 0.2719(8) 0.4549(6) 0.1364(8) 0.033(2) Uani 1 1 d . . . . .
O4 O 0.2652(7) 0.3982(4) 0.0993(7) 0.050(2) Uani 1 1 d . . . . .
C5 C 0.1136(8) 0.5437(6) 0.1579(8) 0.033(2) Uani 1 1 d . . . . .
O5 O 0.0114(6) 0.5452(5) 0.1203(6) 0.056(2) Uani 1 1 d . . . . .
C6 C 0.2708(8) 0.5998(5) 0.0805(7) 0.031(2) Uani 1 1 d . . . . .
O6 O 0.2643(7) 0.6332(5) 0.0019(6) 0.055(2) Uani 1 1 d . . . . .
Fe3 Fe 0.64127(11) 0.47413(6) 0.26722(10) 0.0201(2) Uani 1 1 d . . . . .
C7 C 0.2705(8) 0.7304(4) 0.5112(8) 0.0268(18) Uani 1 1 d . . . . .
O7 O 0.1855(7) 0.7582(4) 0.5118(6) 0.0419(18) Uani 1 1 d . . . . .
C8 C 0.4837(9) 0.7139(5) 0.6582(8) 0.032(2) Uani 1 1 d . . . . .
O8 O 0.5228(7) 0.7275(5) 0.7555(6) 0.055(2) Uani 1 1 d . . . . .
C9 C 0.4468(9) 0.7765(5) 0.4485(8) 0.031(2) Uani 1 1 d . . . . .
O9 O 0.4698(7) 0.8293(3) 0.4171(6) 0.0448(18) Uani 1 1 d . . . . .
Fe4 Fe 0.40992(11) 0.69455(6) 0.50694(10) 0.0214(2) Uani 1 1 d . . . . .
C10 C 0.5385(9) 0.4412(5) 0.1325(8) 0.031(2) Uani 1 1 d . . . . .
O10 O 0.4793(7) 0.4217(4) 0.0419(6) 0.0481(19) Uani 1 1 d . . . . .
C11 C 0.7215(8) 0.5338(5) 0.2053(8) 0.0303(19) Uani 1 1 d . . . . .
O11 O 0.7746(7) 0.5709(4) 0.1674(6) 0.0474(19) Uani 1 1 d . . . . .
C12 C 0.7274(9) 0.3942(5) 0.2777(8) 0.033(2) Uani 1 1 d . . . . .
O12 O 0.7773(7) 0.3413(4) 0.2774(6) 0.0405(17) Uani 1 1 d . . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
I1 Ge5 2.6714(11) . ?
I2 Ge3 2.7853(10) . ?
I2 Ge4 2.8604(10) . ?
Ge1 Fe1 2.4578(14) . ?
Ge1 Fe2 2.4587(14) 3_666 ?
Ge1 Ge2 2.5971(12) 3_666 ?
Ge1 Ge5 2.7029(12) . ?
Ge1 Ge6 2.7672(13) 3_666 ?
Ge1 Ge4 2.9291(12) . ?
Ge2 Fe3 2.4500(13) . ?
Ge2 Fe4 2.4581(14) 3_666 ?
Ge2 Ge1 2.5971(12) 3_666 ?
Ge2 Ge5 2.7173(13) . ?
Ge2 Ge6 2.7851(13) 3_666 ?
Ge3 Fe3 2.3893(14) . ?
Ge3 Fe2 2.4322(15) . ?
Ge3 Ge4 2.5195(12) . ?
Ge4 Fe1 2.3826(15) . ?
Ge4 Fe4 2.4293(14) . ?
Ge4 Ge6 2.9210(13) . ?
Ge5 Fe3 2.3444(14) . ?
Ge5 Fe1 2.3453(15) . ?
Ge6 Fe2 2.3011(15) . ?
Ge6 Fe4 2.3042(15) . ?
Ge6 Ge1 2.7672(13) 3_666 ?
Ge6 Ge2 2.7852(13) 3_666 ?
Fe1 C3 1.765(9) . ?
Fe1 C1 1.795(9) . ?
Fe1 C2 1.798(10) . ?
C1 O1 1.144(10) . ?
C2 O2 1.136(11) . ?
C3 O3 1.152(10) . ?
Fe2 C4 1.784(10) . ?
Fe2 C5 1.796(9) . ?
Fe2 C6 1.797(9) . ?
Fe2 Ge1 2.4587(14) 3_666 ?
C4 O4 1.136(11) . ?
C5 O5 1.135(11) . ?
C6 O6 1.121(10) . ?
Fe3 C10 1.776(9) . ?
Fe3 C12 1.779(10) . ?
Fe3 C11 1.789(9) . ?
C7 O7 1.133(10) . ?
C7 Fe4 1.799(9) . ?
C8 O8 1.141(10) . ?
C8 Fe4 1.778(9) . ?
C9 O9 1.119(10) . ?
C9 Fe4 1.797(9) . ?
Fe4 Ge2 2.4582(14) 3_666 ?
C10 O10 1.141(11) . ?
C11 O11 1.134(10) . ?
C12 O12 1.146(11) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
Ge3 I2 Ge4 52.99(3) . . ?
Fe1 Ge1 Fe2 125.63(5) . 3_666 ?
Fe1 Ge1 Ge2 111.53(5) . 3_666 ?
Fe2 Ge1 Ge2 108.26(4) 3_666 3_666 ?
Fe1 Ge1 Ge5 53.81(4) . . ?
Fe2 Ge1 Ge5 122.05(5) 3_666 . ?
Ge2 Ge1 Ge5 125.71(4) 3_666 . ?
Fe1 Ge1 Ge6 129.88(5) . 3_666 ?
Fe2 Ge1 Ge6 51.84(4) 3_666 3_666 ?
Ge2 Ge1 Ge6 115.49(4) 3_666 3_666 ?
Ge5 Ge1 Ge6 84.35(4) . 3_666 ?
Fe1 Ge1 Ge4 51.60(4) . . ?
Fe2 Ge1 Ge4 165.09(5) 3_666 . ?
Ge2 Ge1 Ge4 65.22(3) 3_666 . ?
Ge5 Ge1 Ge4 69.73(3) . . ?
Ge6 Ge1 Ge4 142.78(4) 3_666 . ?
Fe3 Ge2 Fe4 124.71(5) . 3_666 ?
Fe3 Ge2 Ge1 112.69(5) . 3_666 ?
Fe4 Ge2 Ge1 108.77(4) 3_666 3_666 ?
Fe3 Ge2 Ge5 53.66(4) . . ?
Fe4 Ge2 Ge5 121.31(5) 3_666 . ?
Ge1 Ge2 Ge5 125.65(4) 3_666 . ?
Fe3 Ge2 Ge6 128.70(5) . 3_666 ?
Fe4 Ge2 Ge6 51.68(4) 3_666 3_666 ?
Ge1 Ge2 Ge6 115.46(4) 3_666 3_666 ?
Ge5 Ge2 Ge6 83.74(4) . 3_666 ?
Fe3 Ge3 Fe2 126.93(5) . . ?
Fe3 Ge3 Ge4 112.28(5) . . ?
Fe2 Ge3 Ge4 113.10(5) . . ?
Fe3 Ge3 I2 112.55(4) . . ?
Fe2 Ge3 I2 110.53(4) . . ?
Ge4 Ge3 I2 65.03(3) . . ?
Fe1 Ge4 Fe4 126.17(5) . . ?
Fe1 Ge4 Ge3 113.44(5) . . ?
Fe4 Ge4 Ge3 115.41(5) . . ?
Fe1 Ge4 I2 111.34(4) . . ?
Fe4 Ge4 I2 110.49(4) . . ?
Ge3 Ge4 I2 61.98(3) . . ?
Fe1 Ge4 Ge6 156.10(5) . . ?
Fe4 Ge4 Ge6 49.99(4) . . ?
Ge3 Ge4 Ge6 65.49(3) . . ?
I2 Ge4 Ge6 89.62(3) . . ?
Fe1 Ge4 Ge1 53.94(4) . . ?
Fe4 Ge4 Ge1 99.77(4) . . ?
Ge3 Ge4 Ge1 95.66(4) . . ?
I2 Ge4 Ge1 147.83(4) . . ?
Ge6 Ge4 Ge1 102.18(4) . . ?
Fe3 Ge5 Fe1 137.77(6) . . ?
Fe3 Ge5 I1 110.60(5) . . ?
Fe1 Ge5 I1 111.63(5) . . ?
Fe3 Ge5 Ge1 118.91(5) . . ?
Fe1 Ge5 Ge1 57.75(4) . . ?
I1 Ge5 Ge1 94.30(4) . . ?
Fe3 Ge5 Ge2 57.33(4) . . ?
Fe1 Ge5 Ge2 118.72(5) . . ?
I1 Ge5 Ge2 94.46(4) . . ?
Ge1 Ge5 Ge2 66.19(3) . . ?
Fe2 Ge6 Fe4 157.52(6) . . ?
Fe2 Ge6 Ge1 57.15(4) . 3_666 ?
Fe4 Ge6 Ge1 119.95(5) . 3_666 ?
Fe2 Ge6 Ge2 120.15(5) . 3_666 ?
Fe4 Ge6 Ge2 56.82(4) . 3_666 ?
Ge1 Ge6 Ge2 64.42(3) 3_666 3_666 ?
Fe2 Ge6 Ge4 103.97(5) . . ?
Fe4 Ge6 Ge4 53.85(4) . . ?
Ge1 Ge6 Ge4 90.24(4) 3_666 . ?
Ge2 Ge6 Ge4 63.18(3) 3_666 . ?
C3 Fe1 C1 97.3(4) . . ?
C3 Fe1 C2 94.2(4) . . ?
C1 Fe1 C2 97.4(4) . . ?
C3 Fe1 Ge5 166.0(3) . . ?
C1 Fe1 Ge5 94.6(3) . . ?
C2 Fe1 Ge5 91.6(3) . . ?
C3 Fe1 Ge4 86.1(3) . . ?
C1 Fe1 Ge4 92.5(3) . . ?
C2 Fe1 Ge4 170.0(3) . . ?
Ge5 Fe1 Ge4 86.01(5) . . ?
C3 Fe1 Ge1 98.2(3) . . ?
C1 Fe1 Ge1 158.9(3) . . ?
C2 Fe1 Ge1 95.7(3) . . ?
Ge5 Fe1 Ge1 68.44(4) . . ?
Ge4 Fe1 Ge1 74.46(4) . . ?
O1 C1 Fe1 178.6(9) . . ?
O2 C2 Fe1 177.1(8) . . ?
O3 C3 Fe1 175.5(8) . . ?
C4 Fe2 C5 92.1(4) . . ?
C4 Fe2 C6 101.5(4) . . ?
C5 Fe2 C6 91.9(4) . . ?
C4 Fe2 Ge6 152.6(3) . . ?
C5 Fe2 Ge6 94.0(3) . . ?
C6 Fe2 Ge6 105.0(3) . . ?
C4 Fe2 Ge3 97.7(3) . . ?
C5 Fe2 Ge3 170.2(3) . . ?
C6 Fe2 Ge3 85.7(3) . . ?
Ge6 Fe2 Ge3 77.43(5) . . ?
C4 Fe2 Ge1 81.7(3) . 3_666 ?
C5 Fe2 Ge1 105.1(3) . 3_666 ?
C6 Fe2 Ge1 162.7(3) . 3_666 ?
Ge6 Fe2 Ge1 71.01(4) . 3_666 ?
Ge3 Fe2 Ge1 76.96(4) . 3_666 ?
O4 C4 Fe2 175.8(8) . . ?
O5 C5 Fe2 173.3(8) . . ?
O6 C6 Fe2 176.1(9) . . ?
C10 Fe3 C12 88.3(4) . . ?
C10 Fe3 C11 96.7(4) . . ?
C12 Fe3 C11 99.7(4) . . ?
C10 Fe3 Ge5 173.1(3) . . ?
C12 Fe3 Ge5 95.3(3) . . ?
C11 Fe3 Ge5 88.6(3) . . ?
C10 Fe3 Ge3 88.2(3) . . ?
C12 Fe3 Ge3 164.5(3) . . ?
C11 Fe3 Ge3 95.7(3) . . ?
Ge5 Fe3 Ge3 86.75(5) . . ?
C10 Fe3 Ge2 105.1(3) . . ?
C12 Fe3 Ge2 91.0(3) . . ?
C11 Fe3 Ge2 156.0(3) . . ?
Ge5 Fe3 Ge2 69.01(4) . . ?
Ge3 Fe3 Ge2 75.35(4) . . ?
O7 C7 Fe4 174.6(8) . . ?
O8 C8 Fe4 175.0(9) . . ?
O9 C9 Fe4 176.5(9) . . ?
C8 Fe4 C9 98.1(4) . . ?
C8 Fe4 C7 91.1(4) . . ?
C9 Fe4 C7 93.0(4) . . ?
C8 Fe4 Ge6 151.6(3) . . ?
C9 Fe4 Ge6 110.1(3) . . ?
C7 Fe4 Ge6 90.6(3) . . ?
C8 Fe4 Ge4 104.9(3) . . ?
C9 Fe4 Ge4 83.5(3) . . ?
C7 Fe4 Ge4 164.0(3) . . ?
Ge6 Fe4 Ge4 76.16(5) . . ?
C8 Fe4 Ge2 81.2(3) . 3_666 ?
C9 Fe4 Ge2 157.9(3) . 3_666 ?
C7 Fe4 Ge2 109.1(3) . 3_666 ?
Ge6 Fe4 Ge2 71.50(5) . 3_666 ?
Ge4 Fe4 Ge2 75.47(4) . 3_666 ?
O10 C10 Fe3 174.4(9) . . ?
O11 C11 Fe3 178.6(9) . . ?
O12 C12 Fe3 175.4(9) . . ?
 
_refine_diff_density_max    1.087
_refine_diff_density_min   -1.039
_refine_diff_density_rms    0.250

_shelxl_version_number 2013-2



