Aluminylation: a generalizable route towards low-valent aluminum under moderate conditions with controlled product nuclearity through precursor design
Reuel, Paris C.; Shandilya, Yogesh; Wattoo, M. Talha; Altman, Alison B.; Chemical Science  (2026) –; doi:10.1039/D6SC02187E

data_1577082
_publ_section_title
;
 Aluminylation: a generalizable route towards low-valent aluminum under
 moderate conditions with controlled product nuclearity through precursor
 design.
;
_journal_issue                   20
_journal_name_full               'Chemical science'
_journal_page_first              10251
_journal_page_last               10259
_journal_paper_doi               10.1039/d6sc02187e
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'C50 H82 Al4 N2 Si2, 1.005(C6 H14)'
_chemical_formula_sum            'C56.03 H96.07 Al4 N2 Si2'
_chemical_formula_weight         961.87
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2qyrt8
_audit_creation_date             2026-02-02
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-02-13 deposited with the CCDC.	2026-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.065(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1442(9)
_cell_length_b                   16.3268(10)
_cell_length_c                   22.4903(15)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      68.38
_cell_measurement_theta_min      3.86
_cell_volume                     5894.9(6)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.948
_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_unetI/netI     0.0809
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5270
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.449
_diffrn_reflns_theta_min         3.861
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.375
_exptl_absorpt_correction_T_max  0.753055
_exptl_absorpt_correction_T_min  0.623312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0950 before and 0.0695 after correction.
 
For component 2:
 wR2(int) was 0.1084 before and 0.0671 after correction.

Final HKLF 4 output contains 23997 reflections, Rint = 0.0968
 (10066 with I > 3sig(I), Rint = 0.0729)
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.084
_exptl_crystal_description       plate
_exptl_crystal_F_000             2105
_exptl_crystal_size_max          0.367
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         5270
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0803
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0793P)^2^+36.1505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1915
_refine_ls_wR_factor_ref         0.2232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3959
_reflns_number_total             5270
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6sc02187e2.cif
_cod_data_source_block           pcr_2025_185_twin_a
_cod_depositor_comments
'Adding full bibliography for 1577082--1577086.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1577082
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.632
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.58777
 0.41223
2. Rigid body (RIGU) restrains
 C4, C5, C6, C7, C9, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C5)=Sof(H5A)=
 Sof(H5B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C7)=
 Sof(H7A)=Sof(H7B)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C121(H121), C161(H161)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C5(H5A,H5B), C8(H8A,H8B), C7(H7A,H7B)
4.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C13(H13)
4.d Idealised Me refined as rotating group:
 C241(H24A,H24B,H24C), C231(H23A,H23B,H23C), C122(H12A,H12B,H12C), C1(H1A,H1B,
 H1C), C123(H12D,H12E,H12F), C2(H2A,H2B,H2C), C251(H25A,H25B,H25C), C163(H16A,
 H16B,H16C), C3(H3A,H3B,H3C), C211(H21A,H21B,H21C), C162(H16D,H16E,H16F),
 C221(H22A,H22B,H22C), C4(H4A,H4B,H4C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              5461
_olex2_submission_special_instructions 'No special instructions were received'