Aluminum dihydride from E(IV) precursors (E = Si, Ge) and its bond-activation reactivities.
Kumar, Hemant; Kelley, Steven P.; Batra, Tanya; Nagendran, Selvarajan; Walensky, Justin R.; Dalton transactions (Cambridge, England : 2003)  (2026) –; doi:10.1039/d6dt00474a

data_7720848
_publ_section_title
;
 Aluminum dihydride from E(IV) precursors (E = Si, Ge) and its
 bond-activation reactivities.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6453
_journal_page_last               6461
_journal_paper_doi               10.1039/d6dt00474a
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C30 H46 Al2 N4 Se2'
_chemical_formula_sum            'C30 H46 Al2 N4 Se2'
_chemical_formula_weight         674.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-12-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2026-02-19 deposited with the CCDC.	2026-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.708(5)
_cell_length_b                   16.543(6)
_cell_length_c                   17.501(6)
_cell_measurement_reflns_used    8809
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      2.43
_cell_volume                     3390(2)
_computing_cell_refinement       'Bruker Apex4 V.2022.1-1/SAINT V8.40B'
_computing_data_collection       'Bruker Apex4 V.2022.1-1'
_computing_data_reduction        'Bruker Apex4 V.2022.1-1/SAINT V8.40B'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Photon II CMOS area detector'
_diffrn_measurement_method       'shutterless omega and phi scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            103492
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.090
_diffrn_reflns_theta_min         2.327
_diffrn_source                   'Incoatec IMuS microfocus Mo tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.257
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3712
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0475P)^2^+3.9639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.1203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2564
_reflns_number_total             3712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00474a2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7720842--7720848.cif.'
_cod_database_code               7720848
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.823
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9'-C8 \\sim C9-C8
 with sigma of 0.02
 C9'-C11' \\sim C9-C11
 with sigma of 0.02
 C9-C10' \\sim C10-C9'
 with sigma of 0.02
 C15-C13 \\sim C13-C15' \\sim C13-C14' \\sim C14-C13
 with sigma of 0.02
3. Others
 Sof(H8BC)=Sof(H8BD)=Sof(C9')=Sof(H9')=Sof(C10')=Sof(H10A)=Sof(H10B)=Sof(H10C)=
 Sof(C11')=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(1)
 Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10D)=Sof(H10E)=Sof(H10F)=
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(1)
 Fixed Sof: H13A(0.5) H13(0.5) C14(0.5) H14D(0.5) H14E(0.5) H14F(0.5)
 C14'(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C15(0.5) H15D(0.5) H15E(0.5) H15F(0.5)
 C15'(0.5) H15A(0.5) H15B(0.5) H15C(0.5)
4.a Ternary CH refined with riding coordinates:
 C9(H9), C9'(H9'), C13(H13A), C13(H13)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C8(H8BC,H8BD), C12(H12A,H12B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7)
4.d Idealised Me refined with riding coordinates:
 C10(H10D,H10E,H10F), C10'(H10A,H10B,H10C), C11(H11A,H11B,H11C), C11'(H11D,
 H11E,H11F), C14(H14D,H14E,H14F), C14'(H14A,H14B,H14C), C15(H15D,H15E,H15F),
 C15'(H15A,H15B,H15C)
;
_shelx_res_checksum              79425
_olex2_submission_special_instructions 'No special instructions were received'