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_7720847
_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         'C15 H23 Al Cl2 N2'
_chemical_formula_sum            'C15 H23 Al Cl2 N2'
_chemical_formula_weight         329.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   calc
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2026-02-05
_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                 108.115(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1830(7)
_cell_length_b                   8.9346(4)
_cell_length_c                   15.4846(8)
_cell_measurement_reflns_used    9787
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      28.230
_cell_measurement_theta_min      2.667
_cell_volume                     1733.45(15)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0573
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42793
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.278
_diffrn_reflns_theta_min         1.777
_diffrn_source                   'Incoatec IMuS microfocus Mo tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.418
_exptl_absorpt_correction_T_max  0.7090
_exptl_absorpt_correction_T_min  0.6359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       prism
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4283
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0347P)^2^+0.8823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0904
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3644
_reflns_number_total             4283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00474a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7720842--7720848.cif.'
_cod_database_code               7720847
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.936
_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
 C12'-C13' \\sim C13-C12
 with sigma of 0.02
 C15-C12 \\sim C15'-C12'
 with sigma of 0.02
 C12-C11 \\sim C12'-C11
 with sigma of 0.02
3. Others
 Sof(H11C)=Sof(H11D)=Sof(C12')=Sof(H12')=Sof(C13')=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(C15')=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C12(H12), C12'(H12')
4.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C11(H11C,H11D)
4.c Idealised Me refined with riding coordinates:
 C13'(H13D,H13E,H13F), C15'(H15D,H15E,H15F)
4.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              70326
_olex2_submission_special_instructions 'No special instructions were received'