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_1577083
_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         'C62 H94 Li2 N4 O'
_chemical_formula_sum            'C62 H94 Li2 N4 O'
_chemical_formula_weight         925.29
_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
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2qyrwb
_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                74.173(3)
_cell_angle_beta                 86.035(3)
_cell_angle_gamma                86.570(4)
_cell_formula_units_Z            2
_cell_length_a                   10.8117(6)
_cell_length_b                   14.0773(8)
_cell_length_c                   19.9743(11)
_cell_measurement_reflns_used    7651
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      68.33
_cell_measurement_theta_min      3.27
_cell_volume                     2915.2(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 0.969
_diffrn_measured_fraction_theta_max 0.964
_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  0.0405
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24662
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.608
_diffrn_reflns_theta_min         3.266
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6155
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1067 before and 0.0767 after correction.
The Ratio of minimum to maximum transmission is 0.8173.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.054
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.341
_exptl_crystal_size_min          0.293
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0007(2)
_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   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         10348
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.0938
_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^)+(0.1046P)^2^+5.4440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2276
_refine_ls_wR_factor_ref         0.2717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7083
_reflns_number_total             10348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6sc02187e2.cif
_cod_data_source_block           trip_pcr_2025_171_a
_cod_depositor_comments
'Adding full bibliography for 1577082--1577086.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1577083
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.851
_olex2_refinement_description
;
1. Restrained distances
 C161-C163 \\sim C161-C164
 with sigma of 0.02
2. Others
 Sof(H16A)=Sof(C164)=Sof(H16H)=Sof(H16I)=Sof(H16J)=1-FVAR(1)
 Sof(H161)=Sof(C163)=Sof(H16E)=Sof(H16F)=Sof(H16G)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C121(H121), C361(H361), C221(H221), C461(H461), C161(H161), C161(H16A),
 C421(H421), C261(H261), C321(H321)
3.b Secondary CH2 refined with riding coordinates:
 C112(H11A,H11B), C212(H21A,H21B), C113(H11C,H11D), C114(H11E,H11F), C4(H4A,
 H4B), C213(H21C,H21D), C1(H1A,H1B), C3(H3A,H3B), C214(H21E,H21F), C2(H2A,H2B)
3.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C45(H45), C44(H44), C15(H15), C43(H43), C35(H35), C14(H14),
 C23(H23), C33(H33), C24(H24), C25(H25), C34(H34)
3.d Idealised Me refined as rotating group:
 C462(H46A,H46B,H46C), C423(H42A,H42B,H42C), C362(H36A,H36B,H36C), C223(H22A,
 H22B,H22C), C115(H11G,H11H,H11I), C122(H12A,H12B,H12C), C463(H46D,H46E,H46F),
 C123(H12D,H12E,H12F), C262(H26A,H26B,H26C), C363(H36D,H36E,H36F), C222(H22D,
 H22E,H22F), C263(H26D,H26E,H26F), C422(H42D,H42E,H42F), C162(H16B,H16C,H16D),
 C322(H32A,H32B,H32C), C323(H32D,H32E,H32F), C215(H21G,H21H,H21I), C163(H16E,
 H16F,H16G), C164(H16H,H16I,H16J)
;
_shelx_res_checksum              63570
_olex2_submission_special_instructions 'No special instructions were received'