Persilylation of Ferrocene: The Ultimate Discipline in Sterically Overcrowded Metal Complexes
Rupf, Susanne M.; Sievers, Robin; Riemann, Paulin S.; Reimann, Marc; Kaupp, Martin; Fasting, Dr. Carlo; Malischewski, Moritz; Dalton Transactions  (2023) –; doi:10.1039/D3DT01133J

data_7712839
_publ_section_title
;
 Persilylation of Ferrocene: The Ultimate Discipline in Sterically
 Overcrowded Metal Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01133J
_journal_year                    2023
_chemical_formula_moiety         'C26 H58 Fe Si8'
_chemical_formula_sum            'C26 H58 Fe Si8'
_chemical_formula_weight         651.29
_chemical_name_systematic        4b
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-12
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2023-03-12 deposited with the CCDC.	2023-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.4200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.7412(7)
_cell_length_b                   20.9752(7)
_cell_length_c                   19.7446(7)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.347
_cell_measurement_theta_min      2.232
_cell_volume                     7557.8(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            85274
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.402
_diffrn_reflns_theta_min         1.855
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1039 before and 0.0707 after correction.
The Ratio of minimum to maximum transmission is 0.9026.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       plate
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         13874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+4.1466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1287
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9769
_reflns_number_total             13874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01133j2.cif
_cod_data_source_block           test2
_cod_database_code               7712839
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.840
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All Si(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 Si1(H1), Si2(H2), Si12(H12), Si13(H13), Si14(H14), Si15(H15), Si16(H16),
 Si17(H17), Si18(H18), Si19(H19), Si22(H22), Si23(H23), Si24(H24), Si25(H25),
 Si26(H26), Si27(H27)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C19(H19A), C20(H20), C29(H29)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C120(H12A,H12B,H12C), C121(H12D,H12E,H12F),
 C130(H13A,H13B,H13C), C131(H13D,H13E,H13F), C140(H14A,H14B,H14C), C141(H14D,
 H14E,H14F), C150(H15A,H15B,H15C), C151(H15D,H15E,H15F), C160(H16A,H16B,H16C),
 C161(H16D,H16E,H16F), C170(H17A,H17B,H17C), C171(H17D,H17E,H17F), C180(H18A,
 H18B,H18C), C181(H18D,H18E,H18F), C190(H19B,H19C,H19D), C191(H19E,H19F,H19G),
 C220(H22A,H22B,H22C), C221(H22D,H22E,H22F), C230(H23A,H23B,H23C), C231(H23D,
 H23E,H23F), C240(H24A,H24B,H24C), C241(H24D,H24E,H24F), C250(H25A,H25B,H25C),
 C251(H25D,H25E,H25F), C260(H26A,H26B,H26C), C261(H26D,H26E,H26F), C270(H27A,
 H27B,H27C), C271(H27D,H27E,H27F), C280(H28A,H28B,H28C), C281(H28D,H28E,H28F)
;
_shelx_res_checksum              9966
_olex2_submission_special_instructions 'No special instructions were received'