Reductive elimination of [AlH<sub>2</sub>]<sup>+</sup> from a cationic Ga-Al dihydride.
Morris, Louis J.; Carpentier, Ambre; Maron, Laurent; Okuda, Jun; Chemical communications (Cambridge, England) 57 (2021) 9454–9457; doi:10.1039/d1cc03706d

data_7128814
_publ_section_title
;
 Reductive elimination of [AlH<sub>2</sub>]<sup>+</sup> from a cationic
 Ga-Al dihydride.
;
_journal_issue                   74
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9454
_journal_page_last               9457
_journal_paper_doi               10.1039/d1cc03706d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         '2(C43 H67 Al2 N6), 2(C32 H36 B), C7 H8'
_chemical_formula_sum            'C157 H214 Al4 B2 N12'
_chemical_formula_weight         2398.93
_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   mixed
_audit_creation_date             2021-07-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-09 deposited with the CCDC.	2021-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                96.05(3)
_cell_angle_beta                 102.03(3)
_cell_angle_gamma                108.20(3)
_cell_formula_units_Z            1
_cell_length_a                   12.130(2)
_cell_length_b                   16.522(3)
_cell_length_c                   20.716(4)
_cell_measurement_reflns_used    69156
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.43
_cell_measurement_theta_min      2.22
_cell_volume                     3791.9(16)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'Hybrid Pixel Counting Detector'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       '4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            94792
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.134
_diffrn_reflns_theta_min         2.218
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_target            Cu
_diffrn_source_type              'Xenocs Cu microfocus tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  0.7511
_exptl_absorpt_correction_T_min  0.2652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens 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.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.051
_exptl_crystal_description       Block
_exptl_crystal_F_000             1302
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.297
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.00195(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     860
_refine_ls_number_reflns         14496
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0942P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1402
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10438
_reflns_number_total             14496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03706d2.cif
_cod_data_source_block           4Al
_cod_depositor_comments
'Adding full bibliography for 7128813--7128817.cif.'
_cod_original_cell_volume        3791.8(15)
_cod_database_code               7128814
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.745
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C82-C76
 1.51 with sigma of 0.02
 C76-C77 = C76-C81 = C78-C79
 1.39 with sigma of 0.02
 C77-C78 = C79-C80 = C80-C81
 1.38 with sigma of 0.02
 C76-C78
 2.42 with sigma of 0.04
 C77-C79
 2.39 with sigma of 0.04
 C76-C80
 2.41 with sigma of 0.04
 C78-C80 = C79-C81
 2.4 with sigma of 0.04
 C82-C77 = C82-C81
 2.52 with sigma of 0.04
 C76-C77 \\sim C77-C78 \\sim C78-C79 \\sim C79-C80 \\sim C80-C81 \\sim C81-C76
 with sigma of 0.02
 C76-C80 \\sim C76-C78 \\sim C81-C79 \\sim C77-C81 \\sim C78-C80 \\sim C77-C79
 with sigma of 0.04
 C82-C81 \\sim C82-C77
 with sigma of 0.04
3. Restrained planarity
 C76, C77, C78, C79, C80, C81, C82
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81 \\sim C82: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C76, C77, C78, C79, C80, C81, C82
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C76(0.5) C77(0.5) H77(0.5) C78(0.5) H78(0.5) C79(0.5) H79(0.5)
 C80(0.5) H80(0.5) C81(0.5) H81(0.5) C82(0.5) H82A(0.5) H82B(0.5) H82C(0.5)
7.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
7.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C45(H45), C47(H47),
 C49(H49), C53(H53), C55(H55), C57(H57), C61(H61), C63(H63), C65(H65), C69(H69),
  C71(H71), C73(H73), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81)
7.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C33(H33A,
 H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C),
 C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C66(H66A,
 H66B,H66C), C67(H67A,H67B,H67C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C),
 C82(H82A,H82B,H82C)
;
_shelx_res_checksum              1431
_olex2_submission_special_instructions 'No special instructions were received'