Al(II) Transfer Harnessing a Well-Defined Cadmium Precursor
Herle, Dominic; Wurm, Frerik; Lichtenberg, Crispin; Dankert, Fabian Maurice; Chemical Science  (2026) –; doi:10.1039/D6SC00437G

data_1576638
_publ_section_title
;
 Al(ii) transfer harnessing a well-defined cadmium precursor.
;
_journal_issue                   16
_journal_name_full               'Chemical science'
_journal_page_first              7997
_journal_page_last               8006
_journal_paper_doi               10.1039/d6sc00437g
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         '2(C11 H23 Al0.5 N1.5 O Si)'
_chemical_formula_sum            'C22 H46 Al N3 O2 Si2'
_chemical_formula_weight         467.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-12-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-12-16 deposited with the CCDC.	2026-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 127.024(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8826(6)
_cell_length_b                   10.2863(3)
_cell_length_c                   16.5219(5)
_cell_measurement_reflns_used    23840
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.37
_cell_measurement_theta_min      4.45
_cell_volume                     2697.76(16)
_computing_cell_refinement
;
X-Area Recipe 2.0.1 (STOE, 2023)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.192.0 (STOE, 2023)
;
_computing_data_reduction
;
X-Area Integrate 2.5.15.0 (STOE, 2023)
X-Area LANA 2.7.12 (STOE, 2023)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
 3787 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13804
_diffrn_reflns_point_group_measured_fraction_full 0.873
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        66.954
_diffrn_reflns_theta_max         66.954
_diffrn_reflns_theta_min         3.351
_diffrn_source                   Cu-Genix
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.675
_exptl_absorpt_correction_T_max  0.9514
_exptl_absorpt_correction_T_min  0.7417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 1562 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         4213
_refine_ls_number_restraints     364
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0873P)^2^+1.8391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1366
_reflns_Friedel_coverage         0.647
_reflns_Friedel_fraction_full    0.730
_reflns_Friedel_fraction_max     0.730
_reflns_number_gt                4148
_reflns_number_total             4213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6sc00437g2.cif
_cod_data_source_block           sv1808
_cod_depositor_comments
'Adding full bibliography for 1576637--1576642.cif.'
_cod_original_cell_volume        2697.76(15)
_cod_database_code               1576638
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.57283
 0.42717
2. Restrained distances
 Si2-C20 \\sim Si2-C21 \\sim Si2-C22 \\sim Si2A-C20A \\sim Si2A-C21A \\sim
Si2A-C22A
 with sigma of 0.002
 N3-C12A \\sim N3-C12
 with sigma of 0.02
 Si1-N2 \\sim Si1A-N2
 with sigma of 0.002
 C15A-C16 \\sim C13A-C12A \\sim C17A-C16 \\sim C19A-C12A
 with sigma of 0.002
 C13A-C14A \\sim C15A-C14A \\sim C17A-C18A \\sim C19A-C18A
 with sigma of 0.002
 C17A-C16 \\sim C17-C16 \\sim C15-C16 \\sim C15A-C16
 with sigma of 0.002
 N3A-C12A \\sim N3-C12
 with sigma of 0.002
3. Rigid bond restraints
 N3, C16, C17A, C15A, C13A, C12A, C18A, C14A, C19A, C17, C15, C13, C12, C18,
 C14, C19
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Si2, C20A, C21, C22, Si2A, C20, C22A, C21A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N4, N4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1, C8, C2, C5, C7, C4, C6, C3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C10, H10A, H10B, H10C, C11A, H11A, H11B, H11C, C9A, H9AA, H9AB, H9AC, Si1,
 Si1A, C9, H9A, H9B, H9C, C10A, H10D, H10E, H10F, C11, H11D, H11E, H11F
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(N3) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C15A)
\\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C12A) \\sim Ueq, Uanis(C18A) \\sim Ueq,
Uanis(C14A) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C14) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Si1) \\sim Ueq, Uanis(Si1A) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.002
Uanis(C20A) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C21A)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(Si2A) \\sim Ueq,
Uanis(Si2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C7) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C3)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C11) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(Si1A) \\sim Ueq, Uanis(Si1)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C9A) \\sim Ueq,
Uanis(C10A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C11A) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C10A) \\sim Ueq: with sigma of 0.003 and
sigma for terminal atoms of 0.006
Uanis(Si1A) = Uanis(Si1)
5. Others
 Sof(N3)=Sof(O2)=Sof(H16A)=Sof(C17)=Sof(H17C)=Sof(H17D)=Sof(C15)=Sof(H15C)=
 Sof(H15D)=Sof(C13)=Sof(H13C)=Sof(H13D)=Sof(C12)=Sof(H12)=Sof(C18)=Sof(H18C)=
 Sof(H18D)=Sof(C14)=Sof(H14C)=Sof(H14D)=Sof(C19)=Sof(H19C)=Sof(H19D)=1-FVAR(1)
 Sof(H16)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(C15A)=Sof(H15A)=Sof(H15B)=
 Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(C12A)=Sof(H12A)=Sof(C18A)=Sof(H18A)=
 Sof(H18B)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(N3A)=
 Sof(O2A)=FVAR(1)
 Fixed Sof: Si2(0.5) C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C20A(0.5)
 H20A(0.5) H20B(0.5) H20C(0.5) C11A(0.5) H11A(0.5) H11B(0.5) H11C(0.5) C21(0.5)
 H21A(0.5) H21B(0.5) H21C(0.5) C22(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C9A(0.5)
 H9AA(0.5) H9AB(0.5) H9AC(0.5) Si2A(0.5) C20(0.5) H20D(0.5) H20E(0.5) H20F(0.5)
 C22A(0.5) H22D(0.5) H22E(0.5) H22F(0.5) C21A(0.5) H21D(0.5) H21E(0.5)
 H21F(0.5) N4(0.5) Si1(0.5) Si1A(0.5) C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5)
 C10A(0.5) H10D(0.5) H10E(0.5) H10F(0.5) C11(0.5) H11D(0.5) H11E(0.5) H11F(0.5)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C5(H5), C16(H16A), C16(H16), C12A(H12A), C12(H12)
6.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C2(H2A,H2B), C7(H7A,H7B), C4(H4A,H4B), C6(H6A,H6B), C3(H3A,H3B),
 C17A(H17A,H17B), C15A(H15A,H15B), C13A(H13A,H13B), C18A(H18A,H18B), C14A(H14A,
 H14B), C19A(H19A,H19B), C17(H17C,H17D), C15(H15C,H15D), C13(H13C,H13D),
 C18(H18C,H18D), C14(H14C,H14D), C19(H19C,H19D)
6.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C20A(H20A,H20B,H20C), C11A(H11A,H11B,H11C), C21(H21A,
 H21B,H21C), C22(H22A,H22B,H22C), C9A(H9AA,H9AB,H9AC), C20(H20D,H20E,H20F),
 C22A(H22D,H22E,H22F), C21A(H21D,H21E,H21F), C9(H9A,H9B,H9C), C10A(H10D,H10E,
 H10F), C11(H11D,H11E,H11F)
;
_shelx_res_checksum              39886
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '60.0 mm'
_stoe_detector_pixelsize_x       '0.172 mm'
_stoe_detector_pixelsize_y       '0.172 mm'
_stoe_detector_size_x            '7.0 cm'
_stoe_detector_size_y            '8.4 cm'
_stoe_evaluation_integration_a   8.0
_stoe_evaluation_integration_b   0.0
_stoe_evaluation_integration_ems 0.025
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 85.3
_stoe_evaluation_lana_dxs_max_order 1
_stoe_evaluation_lana_dys_max_order 1
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 143.8
_stoe_evaluation_lana_max_2theta_desired 143.8
_stoe_evaluation_lana_mean_redundancy 3.2
_stoe_evaluation_lana_number_refls_after_or 14563
_stoe_evaluation_lana_number_refls_outliers 4084
_stoe_evaluation_lana_number_refls_total 18647
_stoe_evaluation_lana_number_refls_unique 4526
_stoe_evaluation_lana_number_refls_written 14563
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group 2
_stoe_evaluation_lana_table
;
2Theta          13.7   29.1   44.5   59.9   75.3   90.7  106.1  121.5  136.9
<Resolution>    5.14   2.92   2.03   1.55   1.26   1.08   0.97   0.88   0.83
N(total)          76    531    823   1065   1734   4485   4268   3863   1802
<Redundancy>     1.9    3.0    2.3    2.0    2.1    4.4    4.0    3.7    2.8
Complet. [%%]    92.7   98.7   95.7   89.8   85.9   89.2   86.4   84.4   69.7
<I/sigma>      458.3  184.7   87.1   46.9   34.1   15.6   14.0   11.0    9.6
R(int)         0.007  0.010  0.012  0.013  0.036  0.045  0.044  0.057  0.054
;
_stoe_measurement_identifier     sv1808
_stoe_measurement_max_exposure_per_frame '20.0 s'
_stoe_measurement_mean_exposure_per_frame '20.0 s'
_stoe_measurement_min_exposure_per_frame '20.0 s'
_stoe_measurement_total_exposure_time '21.0 h'
_stoe_measurement_total_frame_number 3787
_stoe_measurement_total_run_number 33
_stoe_measurement_tube_power     '30.0 W'