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_7719845
_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         'C44 H36 Fe4 Ge O4, [+ solvents]'
_chemical_formula_sum            'C44 H36 Fe4 Ge O4'
_chemical_formula_weight         924.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-07-31
_audit_creation_method
;
Olex2 1.5-ac7-014
(compiled 2025.02.27 svn.r6f4c0eaf for Rigaku Oxford Diffraction, GUI svn.r7171)
;
_audit_update_record
;
2025-08-04 deposited with the CCDC.	2025-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.9230(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0890(3)
_cell_length_b                   16.1723(2)
_cell_length_c                   21.2268(4)
_cell_measurement_reflns_used    16040
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.2700
_cell_measurement_theta_min      4.1930
_cell_volume                     4732.22(15)
_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-ac7-014 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-014 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution
'olex2.solve 1.5-ac7-014 (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 0.994
_diffrn_measured_fraction_theta_max 0.978
_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    -51.00 -11.00   0.50    3.00    --    0.00 123.00  80.26   80
  2  \w    -38.00  -6.00   0.50    3.00    --    8.00 115.00 117.56   64
  3  \w      0.00  26.00   0.50    3.00    --   24.00  76.00 -63.33   52
  4  \w   -128.00 -12.00   0.50    3.00    --  -51.57 -19.00 -30.00  232
  5  \w   -139.00 -47.00   0.50    3.00    --  -64.00 -54.00  96.58  184
  6  \w   -105.00 -13.00   0.50    3.00    --  -80.25  77.00-120.00  184
  7  \w    -71.00  -7.00   0.50    3.00    --  -80.25  61.00  90.00  128
  8  \w   -151.00 -87.00   0.50    3.00    --  -80.25-125.00-150.00  128
  9  \w    -51.00  -4.00   0.50    3.00    --  -80.25  45.00 -30.00   94
 10  \w   -105.00 -13.00   0.50    3.00    --  -80.25  77.00  30.00  184
 11  \w    -85.00 -13.00   0.50    3.00    --  -80.25 125.00-150.00  144
 12  \w    -85.00 -13.00   0.50    3.00    --  -80.25 125.00-150.00  144
 13  \w    -35.00  -2.00   0.50    3.00    --  -80.25  30.00-180.00   66
 14  \w   -162.00 -87.00   0.50   12.00    --  -88.50 -59.00  41.66  150
 15  \w     34.00  71.00   0.50   12.00    --  106.74 -61.00  90.00   74
 16  \w     36.00 112.00   0.50   12.00    --  106.74-125.00  90.00  152
 17  \w     34.00  71.00   0.50   12.00    --  106.74 -61.00 120.00   74
 18  \w     36.00 112.00   0.50   12.00    --  106.74-125.00-120.00  152
 19  \w     92.00 178.00   0.50   12.00    --  106.74  45.00  90.00  172
 20  \w     40.00 105.00   0.50   12.00    --  106.74 -95.00  30.00  130
 21  \w     34.00  71.00   0.50   12.00    --  106.74 -61.00-120.00   74
 22  \w    101.00 174.00   0.50   12.00    --  106.74  77.00   0.00  146
 23  \w     40.00 105.00   0.50   12.00    --  106.74 -95.00 120.00  130
 24  \w     40.00 105.00   0.50   12.00    --  106.74 -95.00-120.00  130
 25  \w     90.00 178.00   0.50   12.00    --  106.74  30.00 150.00  176
 26  \w     36.00 112.00   0.50   12.00    --  106.74-125.00-120.00  152
 27  \w     34.00  71.00   0.50   12.00    --  106.74 -61.00 -30.00   74
 28  \w     92.00 178.00   0.50   12.00    --  106.74  45.00 -30.00  172
 29  \w     36.00 112.00   0.50   12.00    --  106.74-125.00  60.00  152
 30  \w     92.00 178.00   0.50   12.00    --  106.74  45.00 -30.00  172
 31  \w     40.00 105.00   0.50   12.00    --  106.74 -95.00 -30.00  130
 32  \w     40.00 105.00   0.50   12.00    --  106.74 -77.00  60.00  130
 33  \w    101.00 174.00   0.50   12.00    --  106.74  77.00-150.00  146
 34  \w     90.00 178.00   0.50   12.00    --  106.74  30.00 -90.00  176
 35  \w     40.00 105.00   0.50   12.00    --  106.74 -77.00 150.00  130
 36  \w     34.00  71.00   0.50   12.00    --  106.74 -61.00 150.00   74
 37  \w     91.00 178.00   0.50   12.00    --  106.74  61.00 120.00  174
 38  \w     40.00 105.00   0.50   12.00    --  106.74 -95.00-150.00  130
 39  \w     36.00 112.00   0.50   12.00    --  106.74-125.00 -30.00  152
 40  \w     41.00 108.00   0.50   12.00    --  110.00-110.00 114.00  134
 41  \w    -48.00 -22.00   0.50    3.00    --  -40.00 -61.00 161.30   52
 42  \w   -143.00 -58.00   0.50    3.00    --  -68.00 -52.00-147.53  170
;
_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      0.0321803000
_diffrn_orient_matrix_UB_12      0.0180631000
_diffrn_orient_matrix_UB_13      -0.0637581000
_diffrn_orient_matrix_UB_21      -0.1066365000
_diffrn_orient_matrix_UB_22      -0.0019763000
_diffrn_orient_matrix_UB_23      -0.0361623000
_diffrn_orient_matrix_UB_31      -0.0084694000
_diffrn_orient_matrix_UB_32      0.0935093000
_diffrn_orient_matrix_UB_33      0.0115171000
_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  0.0621
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35621
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.069
_diffrn_reflns_theta_min         4.214
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.598
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_correction_T_min  0.589
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.106
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         5010
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0891P)^2^+21.1666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1584
_refine_ls_wR_factor_ref         0.1662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4168
_reflns_number_total             5010
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02029h2.cif
_cod_data_source_block           at1608-mk69
_cod_depositor_comments
'Adding full bibliography for 7719844--7719848.cif.'
_cod_original_cell_volume        4732.21(15)
_cod_database_code               7719845
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C43H42GeO5FeCl
_chemical_oxdiff_usercomment     MHX69
_shelx_estimated_absorpt_t_max   0.400
_shelx_estimated_absorpt_t_min   0.242
_diffrn_oxdiff_digest_hkl
;
438e2ef6cc316b32ceaadeecf1ef32e716af5b
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              50004
_shelx_fab_checksum              87224
_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 3.171
_oxdiff_exptl_absorpt_empirical_full_min 0.472