Synthesis, structure, photochemical and electrochemical properties of α-germyl ferrocenyl ketones.
Heurix, Madeleine; Harmach, Petr; Torvisco, Ana; Fischer, Roland C.; Wiech, Mathias; Císařová, Ivana; Gescheidt, Georg; Štěpnička, Petr; Haas, Michael; Dalton transactions (Cambridge, England : 2003) 54 (2025) 17611–17620; doi:10.1039/d5dt02029h

data_7719848
_publ_section_title
;
 Synthesis, structure, photochemical and electrochemical properties of
 &#x3b1;-germyl ferrocenyl ketones.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17611
_journal_page_last               17620
_journal_paper_doi               10.1039/d5dt02029h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C20 H36 Fe Ge O Si3'
_chemical_formula_sum            'C20 H36 Fe Ge O Si3'
_chemical_formula_weight         505.20
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-12-11
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2025-08-04 deposited with the CCDC.	2025-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.27024(4)
_cell_length_b                   18.27024(4)
_cell_length_c                   30.63623(11)
_cell_measurement_reflns_used    138487
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      80.0320
_cell_measurement_theta_min      2.8140
_cell_volume                     10226.42(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.143a 64-bit (release 25-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution
'olex2.solve 1.5-ac6-020 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -48.00  -9.00   0.50    0.50    --    0.00 119.00  83.92   78
  2  \w    -50.00 -10.00   0.50    0.50    --    0.00 121.00-143.25   80
  3  \w    -26.00   7.00   0.50    0.50    --   12.00 100.00  36.43   66
  4  \w    -31.00  -1.00   0.50    0.50    --   12.00 110.00-112.42   60
  5  \w      2.00  30.00   0.50    0.50    --   24.00  73.00  47.25   56
  6  \w     13.00  44.00   0.50    0.50    --   32.00  63.00 103.46   62
  7  \w     17.00  44.00   0.50    0.50    --   36.00  63.00 170.02   54
  8  \w   -139.00 -47.00   0.50    0.50    --  -64.00 -53.00  44.86  184
  9  \w   -139.00 -47.00   0.50    0.50    --  -64.00 -53.00 -42.04  184
 10  \w    -51.00  -4.00   0.50    0.50    --  -80.25  45.00-180.00   94
 11  \w   -147.00-100.00   0.50    0.50    --  -80.25 -95.00  60.00   94
 12  \w   -105.00 -13.00   0.50    0.50    --  -80.25  77.00-150.00  184
 13  \w   -105.00 -13.00   0.50    0.50    --  -80.25  77.00  60.00  184
 14  \w    -35.00  -2.00   0.50    0.50    --  -80.25  30.00 -60.00   66
 15  \w    -51.00  -4.00   0.50    0.50    --  -80.25  45.00 150.00   94
 16  \w    -85.00 -13.00   0.50    0.50    --  -80.25 125.00-120.00  144
 17  \w    -35.00  -2.00   0.50    0.50    --  -80.25  30.00-150.00   66
 18  \w   -162.00 -87.00   0.50    0.50    --  -88.50 -59.00-100.30  150
 19  \w     34.00  71.00   0.50    0.50    --  106.74 -61.00 -30.00   74
 20  \w     34.00  71.00   0.50    0.50    --  106.74 -61.00 150.00   74
 21  \w     34.00  71.00   0.50    0.50    --  106.74 -61.00-150.00   74
 22  \w     36.00 112.00   0.50    0.50    --  106.74-125.00-180.00  152
 23  \w     36.00 112.00   0.50    0.50    --  106.74-125.00-180.00  152
 24  \w     36.00 112.00   0.50    0.50    --  106.74-125.00   0.00  152
 25  \w     40.00 105.00   0.50    0.50    --  106.74 -95.00 -90.00  130
 26  \w     34.00  71.00   0.50    0.50    --  106.74 -61.00  60.00   74
 27  \w     90.00 178.00   0.50    0.50    --  106.74  30.00   0.00  176
 28  \w     40.00 105.00   0.50    0.50    --  106.74 -95.00 -30.00  130
 29  \w     92.00 178.00   0.50    0.50    --  106.74  45.00 120.00  172
 30  \w     99.00 176.00   0.50    0.50    --  106.74 119.00-179.00  154
 31  \w     36.00 112.00   0.50    0.50    --  106.74-125.00-120.00  152
 32  \w     92.00 178.00   0.50    0.50    --  106.74  45.00   0.00  172
 33  \w     40.00 105.00   0.50    0.50    --  106.74 -77.00 120.00  130
 34  \w     34.00  71.00   0.50    0.50    --  106.74 -61.00 120.00   74
 35  \w     90.00 178.00   0.50    0.50    --  106.74  30.00  90.00  176
 36  \w    101.00 174.00   0.50    0.50    --  106.74  77.00 150.00  146
 37  \w     40.00 105.00   0.50    0.50    --  106.74 -77.00 -60.00  130
 38  \w     34.00  71.00   0.50    0.50    --  106.74 -61.00 -60.00   74
 39  \w    101.00 174.00   0.50    0.50    --  106.74  77.00  30.00  146
 40  \w     92.00 178.00   0.50    0.50    --  106.74  45.00 -60.00  172
 41  \w     92.00 178.00   0.50    0.50    --  106.74  45.00   0.00  172
 42  \w     40.00 105.00   0.50    0.50    --  106.74 -95.00 120.00  130
 43  \w    101.00 174.00   0.50    0.50    --  106.74  77.00-120.00  146
 44  \w     36.00 112.00   0.50    0.50    --  106.74-125.00 -30.00  152
 45  \w     39.00 117.00   0.50    0.50    --  110.00-132.00  73.97  156
 46  \w     40.00 111.00   0.50    0.50    --  110.00-124.00  92.53  142
 47  \w     42.00 107.00   0.50    0.50    --  110.00-100.00  88.10  130
 48  \w     41.00 107.00   0.50    0.50    --  110.00-103.00-123.69  132
 49  \w      8.00  37.00   0.50    0.50    --   28.00  67.00 -86.73   58
 50  \w     17.00  44.00   0.50    0.50    --   36.00  63.00 -43.88   54
 51  \w     18.00  50.00   0.50    0.50    --   36.00  60.00  69.94   64
 52  \w     22.00  48.00   0.50    0.50    --   40.00  61.00  -5.41   52
 53  \w    -48.00 -22.00   0.50    0.50    --  -40.00 -61.00 123.76   52
 54  \w   -139.00 -47.00   0.50    0.50    --  -64.00 -54.00 171.89  184
 55  \w   -143.00 -52.00   0.50    0.50    --  -68.00 -52.00 121.54  182
 56  \w   -142.00 -51.00   0.50    0.50    --  -68.00 -56.00-110.47  182
 57  \w   -147.00 -55.00   0.50    0.50    --  -72.00 -55.00  15.94  184
 58  \w   -147.00 -67.00   0.50    0.50    --  -72.00 -54.00 -87.31  160
 59  \w   -155.00 -63.00   0.50    0.50    --  -80.00 -53.00 -62.45  184
 60  \w   -154.00 -63.00   0.50    0.50    --  -80.00 -56.00 -41.08  182
 61  \w   -154.00 -63.00   0.50    0.50    --  -80.00 -56.00-142.43  182
 62  \w   -154.00 -63.00   0.50    0.50    --  -80.00 -56.00 108.52  182
 63  \w   -154.00 -63.00   0.50    0.50    --  -80.00 -56.00  -0.10  182
 64  \w   -154.00 -63.00   0.50    0.50    --  -80.00 -56.00 166.20  182
 65  \w   -154.00 -63.00   0.50    0.50    --  -80.00 -56.00-120.84  182
 66  \w   -159.00 -67.00   0.50    0.50    --  -84.00 -54.00-163.20  184
 67  \w   -159.00 -67.00   0.50    0.50    --  -84.00 -55.00  21.56  184
 68  \w   -163.00 -72.00   0.50    0.50    --  -88.50 -55.00 -78.26  182
 69  \w   -163.00 -72.00   0.50    0.50    --  -88.50 -55.00  95.55  182
 70  \w   -163.00 -72.00   0.50    0.50    --  -88.50 -55.00  61.40  182
 71  \w     92.00 178.00   0.50    0.50    --  106.74  45.00  30.00  172
 72  \w     91.00 178.00   0.50    0.50    --  106.74  61.00 150.00  174
 73  \w     91.00 178.00   0.50    0.50    --  106.74  61.00 120.00  174
 74  \w     91.00 178.00   0.50    0.50    --  106.74  61.00  60.00  174
 75  \w     91.00 178.00   0.50    0.50    --  106.74  61.00 -30.00  174
 76  \w     91.00 178.00   0.50    0.50    --  106.74  61.00-150.00  174
 77  \w     91.00 178.00   0.50    0.50    --  106.74  61.00  30.00  174
 78  \w     91.00 178.00   0.50    0.50    --  106.74  61.00-120.00  174
 79  \w     92.00 178.00   0.50    0.50    --  106.74  45.00-150.00  172
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0344199500
_diffrn_orient_matrix_UB_12      0.0291105500
_diffrn_orient_matrix_UB_13      0.0424856500
_diffrn_orient_matrix_UB_21      0.0502269000
_diffrn_orient_matrix_UB_22      -0.0676461000
_diffrn_orient_matrix_UB_23      0.0020308000
_diffrn_orient_matrix_UB_31      0.0583406000
_diffrn_orient_matrix_UB_32      0.0410527000
_diffrn_orient_matrix_UB_33      -0.0268244000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0067
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            211041
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.502
_diffrn_reflns_theta_min         2.816
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.389
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.199
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.143a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       block
_exptl_crystal_F_000             4224
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.172
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       0.000025(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         5221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0169
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0172P)^2^+8.2498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0422
_refine_ls_wR_factor_ref         0.0423
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5183
_reflns_number_total             5221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02029h2.cif
_cod_data_source_block           at1606-mhx365-at
_cod_depositor_comments
'Adding full bibliography for 7719844--7719848.cif.'
_cod_original_cell_volume        10226.42(6)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7719848
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C43H42GeN2O5FeSi3
_chemical_oxdiff_usercomment     MHX365
_shelx_estimated_absorpt_t_max   0.363
_shelx_estimated_absorpt_t_min   0.240
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,
 H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              69917
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.398
_oxdiff_exptl_absorpt_empirical_full_min 0.697