Redox non-innocent bis-silylene aluminium complexes with a carborane backbone
Saddington, Artemis; Yao, Shenglai; Lorent, Christian; Driess, Matthias; Chemical Science 16 (2025) 6383–6391; doi:10.1039/D5SC01104C

data_1574077
_publ_section_title
;
 Redox non-innocent bis-silylene aluminium complexes with a carborane
 backbone
;
_journal_issue                   15
_journal_name_full               'Chemical Science'
_journal_page_first              6383
_journal_page_last               6391
_journal_paper_doi               10.1039/D5SC01104C
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C32 H56 Al B10 I2 N4 Si2, Al I4, [+ solvents]'
_chemical_formula_sum            'C32 H56 Al2 B10 I6 N4 Si2'
_chemical_formula_weight         1476.44
_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
_audit_creation_date             2025-01-16
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.11.29 svn.rc9064207 for OlexSys, GUI svn.r7097)
;
_audit_update_record
;
2025-01-20 deposited with the CCDC.	2025-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.257(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4094(4)
_cell_length_b                   17.2943(4)
_cell_length_c                   23.7145(6)
_cell_measurement_reflns_used    7870
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      71.6910
_cell_measurement_theta_min      3.1150
_cell_volume                     5905.1(3)
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            42439
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.095
_diffrn_reflns_theta_min         3.164
_exptl_absorpt_coefficient_mu    25.646
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       prism
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         11605
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0582P)^2^+3.5694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8025
_reflns_number_total             11605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01104c2.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 1574073--1574078.cif.'
_cod_database_code               1574077
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.267
_shelx_estimated_absorpt_t_min   0.075
_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. Restrained distances
 I6-Al2 \\sim I6B-Al2 \\sim I5-Al2 \\sim I5B-Al2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
I6 \\sim I5: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
I6B \\sim I5B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
4. Rigid body (RIGU) restrains
 I6, I5, Al2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I6B, Al2, I5B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(I6B)=Sof(I5B)=1-FVAR(1)
 Sof(I6)=Sof(I5)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C24(H24), C20(H20), C23(H23), C21(H21), C6(H6), C10(H10), C8(H8),
 C9(H9A), C7(H7)
6.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C32(H32A,H32B,H32C), C26(H26A,H26B,H26C), C31(H31A,H31B,
 H31C), C12(H12A,H12B,H12C), C18(H18A,H18B,H18C), C28(H28A,H28B,H28C), C30(H30A,
 H30B,H30C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C13(H13A,H13B,H13C),
 C16(H16A,H16B,H16C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 152 electrons were 
found in a volume of 904\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
0.8[C4H10O] per Asymmetric Unit 
which account for 134 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              87455
_shelx_fab_checksum              2737
_olex2_submission_special_instructions 'No special instructions were received'