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_1577085
_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         'C64 H86 Al2 D6 N4, 1[C6H14]'
_chemical_formula_sum            'C70 H100 Al2 D6 N4'
_chemical_formula_weight         1063.58
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2qyrr6
_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                 98.873(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3950(7)
_cell_length_b                   10.6767(7)
_cell_length_c                   24.4982(14)
_cell_measurement_reflns_used    6536
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      67.257
_cell_measurement_theta_min      3.652
_cell_volume                     3203.2(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.979
_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  0.0937
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            36651
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.711
_diffrn_reflns_theta_min         3.785
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1131 before and 0.0840 after correction.
The Ratio of minimum to maximum transmission is 0.8946.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_description       prism
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.185
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.42(10)
_refine_ls_extinction_coef       0.0042(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         11332
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0773
_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^)+(0.0786P)^2^+4.5135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1811
_refine_ls_wR_factor_ref         0.2085
_reflns_Friedel_coverage         0.951
_reflns_Friedel_fraction_full    0.944
_reflns_Friedel_fraction_max     0.933
_reflns_number_gt                7994
_reflns_number_total             11332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6sc02187e2.cif
_cod_data_source_block           mono_pcr_2025_203_a
_cod_depositor_comments
'Adding full bibliography for 1577082--1577086.cif.'
_cod_database_code               1577085
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.848
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.57825
 0.42175
2.a Ternary CH refined with riding coordinates:
 C1(D1), C321(H321), C221(H221), C161(H161), C421(H421), C4(D4), C461(H461),
 C261(H261), C121(H121), C361(H361)
2.b Secondary CH2 refined with riding coordinates:
 C113(H11A,H11B), C112(H11C,H11D), C214(H21A,H21B), C212(H21C,H21D), C114(H11E,
 H11F), C213(H21E,H21F)
2.c Aromatic/amide H refined with riding coordinates:
 C33(H33), C34(H34), C23(H23), C3(D3), C43(H43), C44(H44), C2(D2), C45(H45),
 C5(D5), C6(D6), C35(H35), C15(H15), C24(H24), C13(H13), C14(H14), C25(H25)
2.d Idealised Me refined as rotating group:
 C262(H26A,H26B,H26C), C463(H46A,H46B,H46C), C322(H32A,H32B,H32C), C223(H22A,
 H22B,H22C), C462(H46D,H46E,H46F), C222(H22D,H22E,H22F), C123(H12A,H12B,H12C),
 C362(H36A,H36B,H36C), C215(H21G,H21H,H21I), C423(H42A,H42B,H42C), C363(H36D,
 H36E,H36F), C162(H16A,H16B,H16C), C163(H16D,H16E,H16F), C115(H11G,H11H,H11I),
 C122(H12D,H12E,H12F), C263(H26D,H26E,H26F), C323(H32D,H32E,H32F), C422(H42D,
 H42E,H42F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 98 electrons were 
found in a volume of 478\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C6H14] per Asymmetric Unit 
which account for 100 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              17085
_shelx_fab_checksum              8767
_olex2_submission_special_instructions 'No special instructions were received'