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_7719844
_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 O Si4'
_chemical_formula_sum            'C20 H36 Fe O Si4'
_chemical_formula_weight         460.70
_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     dual
_audit_creation_date             2025-07-31
_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                   18.24740(10)
_cell_length_b                   18.24740(10)
_cell_length_c                   30.4342(3)
_cell_measurement_reflns_used    23165
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      77.3310
_cell_measurement_theta_min      2.8120
_cell_volume                     10133.60(13)
_computing_cell_refinement       'CrysAlisPro 1.171.43.106a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.106a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.106a (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  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(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 0.990
_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     72.00 176.00   0.50    2.00    --  101.05  19.00 -90.00  208
  2  \w    100.00 167.00   0.50    2.00    --  101.05  77.00 -30.00  134
  3  \w     42.00 129.00   0.50    0.50    --   53.17  38.00 -30.00  174
  4  \w     72.00 176.00   0.50    2.00    --  101.05  19.00  60.00  208
  5  \w     72.00 176.00   0.50    2.00    --  101.05  19.00 150.00  208
  6  \w    -21.00  26.00   0.50    0.50    --   53.17 -19.00  60.00   94
  7  \w     36.00 106.00   0.50    2.00    --  101.05 -99.00  30.00  140
  8  \w     35.00 105.00   0.50    2.00    --  101.05 -77.00  30.00  140
  9  \w     36.00 106.00   0.50    2.00    --  101.05 -99.00 -30.00  140
 10  \w     36.00 106.00   0.50    2.00    --  101.05 -99.00 -60.00  140
 11  \w     35.00 105.00   0.50    2.00    --  101.05 -77.00-150.00  140
 12  \w   -127.00 -82.00   0.50    0.50    --  -54.67 -57.00-180.00   90
 13  \w   -127.00 -82.00   0.50    0.50    --  -54.67 -57.00-120.00   90
 14  \w    -43.00  -1.00   0.50    0.50    --  -76.64  38.00 -30.00   84
 15  \w    -43.00  21.00   0.50    0.50    --  -54.67  38.00 -90.00  128
;
_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      0.0291998000
_diffrn_orient_matrix_UB_12      -0.0173049000
_diffrn_orient_matrix_UB_13      -0.0463428000
_diffrn_orient_matrix_UB_21      -0.0384776000
_diffrn_orient_matrix_UB_22      0.0689173000
_diffrn_orient_matrix_UB_23      -0.0179390000
_diffrn_orient_matrix_UB_31      0.0691314000
_diffrn_orient_matrix_UB_32      0.0457542000
_diffrn_orient_matrix_UB_33      0.0096536000
_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  0.0369
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            43158
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.758
_diffrn_reflns_theta_min         2.824
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.632
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.106a (Rigaku Oxford Diffraction, 2024)
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    1.208
_exptl_crystal_description       block
_exptl_crystal_F_000             3936
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0215
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+7.3773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5074
_reflns_number_total             5352
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {d713fd75-a4bb-4c7d-8258-ba0b22394aa4}
_cod_data_source_file            d5dt02029h2.cif
_cod_data_source_block           rf2897_auto
_cod_depositor_comments
'Adding full bibliography for 7719844--7719848.cif.'
_cod_original_cell_volume        10133.61(15)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7719844
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         FeSi4C12H36O2
_shelx_estimated_absorpt_t_max   0.311
_shelx_estimated_absorpt_t_min   0.218
_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 Ternary CH refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C9(H9), C2(H2), C4(H4), C6(H6), C11(H11), C15(H15)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C14(H14A,H14B,H14C), C19(H19A,H19B,
 H19C), C21(H21A,H21B,H21C), C18(H18A,H18B,H18C), C16(H16A,H16B,H16C), C12(H12A,
 H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              45389
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.560
_oxdiff_exptl_absorpt_empirical_full_min 0.536
_publcif_funding_html
;
;