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_7712834
_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 H56 Br2 Fe Si8'
_chemical_formula_sum            'C26 H56 Br2 Fe Si8'
_chemical_formula_weight         809.09
_chemical_name_systematic        1
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-04
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   36.0111(3)
_cell_length_b                   36.0111(3)
_cell_length_c                   12.1108(2)
_cell_measurement_reflns_used    9803
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.28
_cell_measurement_theta_min      2.45
_cell_volume                     15705.3(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            83076
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.276
_diffrn_reflns_theta_min         2.744
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.919
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0895 before and 0.0686 after correction.
The Ratio of minimum to maximum transmission is 0.7054.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       block
_exptl_crystal_F_000             6720
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.164
_refine_diff_density_min         -1.388
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         14394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0761P)^2^+36.2166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12988
_reflns_number_total             14394
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01133j2.cif
_cod_data_source_block           p42_n
_cod_original_cell_volume        15705.3(4)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               7712834
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.275
_shelx_estimated_absorpt_t_min   0.263
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9218(5)
 0.0782(5)
2. Fixed Uiso
 At 1.2 times of:
  All Si(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 Si11(H11), Si12(H12), Si13(H13), Si14(H14), Si16(H16), Si17(H17), Si18(H18),
 Si19(H19), Si21(H21), Si22(H22), Si23(H23), Si24(H24), Si26(H26), Si27(H27),
 Si28(H28), Si29(H29)
3.b Idealised Me refined as rotating group:
 C111(H11D,H11E,H11F), C112(H11A,H11B,H11C), C121(H12D,H12E,H12F), C122(H12A,
 H12B,H12C), C131(H13D,H13E,H13F), C132(H13A,H13B,H13C), C141(H14D,H14E,H14F),
 C142(H14A,H14B,H14C), C161(H16D,H16E,H16F), C162(H16A,H16B,H16C), C171(H17D,
 H17E,H17F), C172(H17A,H17B,H17C), C181(H18D,H18E,H18F), C182(H18A,H18B,H18C),
 C191(H19D,H19E,H19F), C192(H19A,H19B,H19C), C211(H21A,H21B,H21C), C212(H21D,
 H21E,H21F), C221(H22D,H22E,H22F), C222(H22A,H22B,H22C), C231(H23A,H23B,H23C),
 C232(H23D,H23E,H23F), C241(H24A,H24B,H24C), C242(H24D,H24E,H24F), C261(H26D,
 H26E,H26F), C262(H26A,H26B,H26C), C271(H27D,H27E,H27F), C272(H27A,H27B,H27C),
 C281(H28D,H28E,H28F), C282(H28A,H28B,H28C), C291(H29A,H29B,H29C), C292(H29D,
 H29E,H29F)
;
_shelx_res_checksum              92940
_olex2_submission_special_instructions 'No special instructions were received'