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_7712836
_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         'C30 H70 Fe Si10'
_chemical_formula_sum            'C30 H70 Fe Si10'
_chemical_formula_weight         767.61
_chemical_name_systematic        6
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-07
_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                 93.029(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9543(6)
_cell_length_b                   13.4426(7)
_cell_length_c                   13.3587(6)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.28
_cell_volume                     2143.70(18)
_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      100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0765
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            60684
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         2.228
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0821 before and 0.0739 after correction.
The Ratio of minimum to maximum transmission is 0.9488.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+1.4063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3887
_reflns_number_total             4386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01133j2.cif
_cod_data_source_block           p21_n
_cod_database_code               7712836
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.932
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All Si(H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Fe01) = Uanis(C12) = Uanis(C14) = Uanis(C15) = Uanis(C13) = Uanis(C11) =
Uanis(C23) = Uanis(C21) = Uanis(C22) = Uanis(C25) = Uanis(C24)
3. Others
 Fixed Sof: Si11(0.82) H11(0.82) Si12(0.82) H12(0.82) Si13(0.82) H13(0.82)
 Si14(0.82) H14(0.82) Si15(0.82) H15(0.82) Si21(0.18) H21(0.18) Si22(0.18)
 H22(0.18) Si23(0.18) H23(0.18) Si24(0.18) H24(0.18) Si25(0.18) H25(0.18)
 C11(0.82) C12(0.82) C13(0.82) C14(0.82) C15(0.82) C21(0.18) C22(0.18)
 C23(0.18) C24(0.18) C25(0.18) H11G(0.82) H11H(0.82) H11I(0.82) H11J(0.18)
 H11K(0.18) H11L(0.18) H11A(0.82) H11B(0.82) H11C(0.82) H11D(0.18) H11E(0.18)
 H11F(0.18) H12G(0.82) H12H(0.82) H12I(0.82) H12J(0.18) H12K(0.18) H12L(0.18)
 H12A(0.82) H12B(0.82) H12C(0.82) H12D(0.18) H12E(0.18) H12F(0.18) H13J(0.18)
 H13K(0.18) H13L(0.18) H13G(0.82) H13H(0.82) H13I(0.82) H13A(0.82) H13B(0.82)
 H13C(0.82) H13D(0.18) H13E(0.18) H13F(0.18) H14G(0.82) H14H(0.82) H14I(0.82)
 H14J(0.18) H14K(0.18) H14L(0.18) H14A(0.82) H14B(0.82) H14C(0.82) H14D(0.18)
 H14E(0.18) H14F(0.18) H15G(0.82) H15H(0.82) H15I(0.82) H15J(0.18) H15K(0.18)
 H15L(0.18) H15D(0.18) H15E(0.18) H15F(0.18) H15A(0.82) H15B(0.82) H15C(0.82)
4.a Ternary CH refined with riding coordinates:
 Si22(H22), Si24(H24), Si25(H25)
4.b Idealised Me refined as rotating group:
 C111(H11G,H11H,H11I), C111(H11J,H11K,H11L), C112(H11A,H11B,H11C), C112(H11D,
 H11E,H11F), C121(H12G,H12H,H12I), C121(H12J,H12K,H12L), C122(H12A,H12B,H12C),
 C122(H12D,H12E,H12F), C131(H13J,H13K,H13L), C131(H13G,H13H,H13I), C132(H13A,
 H13B,H13C), C132(H13D,H13E,H13F), C141(H14G,H14H,H14I), C141(H14J,H14K,H14L),
 C142(H14A,H14B,H14C), C142(H14D,H14E,H14F), C151(H15G,H15H,H15I), C151(H15J,
 H15K,H15L), C152(H15D,H15E,H15F), C152(H15A,H15B,H15C)
;
_shelx_res_checksum              44330
_olex2_submission_special_instructions 'No special instructions were received'