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_1574075
_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, 2(C7 H8), 2.35[C7H8]'
_chemical_formula_sum            'C46 H72 Al B10 I2 N4 Si2'
_chemical_formula_weight         1126.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-01-17
_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                105.669(4)
_cell_angle_beta                 106.625(5)
_cell_angle_gamma                100.731(4)
_cell_formula_units_Z            2
_cell_length_a                   14.6482(7)
_cell_length_b                   14.8290(7)
_cell_length_c                   18.4781(10)
_cell_measurement_reflns_used    7019
_cell_measurement_temperature    150.2(4)
_cell_measurement_theta_max      72.4460
_cell_measurement_theta_min      3.1970
_cell_volume                     3548.9(4)
_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      150.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.969
_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  0.0611
_diffrn_reflns_av_unetI/netI     0.0738
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26771
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.972
_diffrn_reflns_theta_min         3.230
_exptl_absorpt_coefficient_mu    7.600
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30943
_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    1.054
_exptl_crystal_description       prism
_exptl_crystal_F_000             1146
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.290
_refine_diff_density_min         -1.384
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         13734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0843P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1537
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9866
_reflns_number_total             13734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01104c2.cif
_cod_data_source_block           4a
_cod_depositor_comments
'Adding full bibliography for 1574073--1574078.cif.'
_cod_original_cell_volume        3548.9(3)
_cod_database_code               1574075
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.489
_shelx_estimated_absorpt_t_min   0.326
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C38(H38), C39(H39), C35(H35), C36(H36), C37(H37), C42(H42),
  C43(H43), C44(H44), C45(H45), C46(H46)
2.b Fitted hexagon refined as free rotating group:
 C38(C39,C34,C35,C36,C37)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C40(H40A,H40B,H40C)
2.d Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3), B4(H4), B5(H5A), B6(H6A), B7(H7A), B8(H8A), B9(H9A),
 B10(H10)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 238 electrons were 
found in a volume of 1066\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2.35[C7H8] per Asymmetric Unit 
which account for 235 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              51473
_shelx_fab_checksum              78776
_olex2_submission_special_instructions 'No special instructions were received'