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_7128813
_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         'C14 H34 Al N2 O2, C4 H8 O, C32 H36 B'
_chemical_formula_sum            'C50 H78 Al B N2 O3'
_chemical_formula_weight         792.93
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 117.09(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.966(3)
_cell_length_b                   15.946(3)
_cell_length_c                   12.986(3)
_cell_measurement_reflns_used    46910
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.37
_cell_measurement_theta_min      3.82
_cell_volume                     2390.4(11)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            58430
_diffrn_reflns_point_group_measured_fraction_full 0.670
_diffrn_reflns_point_group_measured_fraction_max 0.653
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.121
_diffrn_reflns_theta_min         3.823
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_description       needle
_exptl_crystal_F_000             868
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF, pentane mixture'
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_coef       0.0012(3)
_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   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         6155
_refine_ls_number_restraints     367
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0743P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1104
_reflns_Friedel_coverage         0.275
_reflns_Friedel_fraction_full    0.317
_reflns_Friedel_fraction_max     0.293
_reflns_number_gt                5296
_reflns_number_total             6155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03706d2.cif
_cod_data_source_block           1thf2
_cod_depositor_comments
'Adding full bibliography for 7128813--7128817.cif.'
_cod_original_cell_volume        2390.6(10)
_cod_database_code               7128813
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1A(0.074) H1B(0.074) H1C(0.074) H2A(0.066) H2B(0.066) H2C(0.066)
 H3A(0.053) H3B(0.053) H4A(0.055) H4B(0.055) H5A(0.079) H5B(0.079) H5C(0.079)
 H6A(0.067) H6B(0.067) H6C(0.067) H7A(0.052) H7B(0.052) H8A(0.048) H8B(0.048)
 H9A(0.046) H9B(0.046) H10A(0.049) H10B(0.049) H11A(0.056) H11B(0.056)
 H12A(0.059) H12B(0.059) H13A(0.062) H13B(0.062) H14A(0.05) H14B(0.05)
 H47A(0.07) H47B(0.07) H48A(0.099) H48B(0.099) H48C(0.099) H48D(0.099)
 H50A(0.101) H50B(0.101) H50C(0.101) H50D(0.101) H49A(0.098) H49B(0.098)
 H49C(0.098) H49D(0.098) H16(0.032) H18(0.036) H20(0.033) H21A(0.055)
 H21B(0.055) H21C(0.055) H22A(0.056) H22B(0.056) H22C(0.056) H24(0.036)
 H26(0.044) H28(0.035) H29A(0.062) H29B(0.062) H29C(0.062) H30A(0.069)
 H30B(0.069) H30C(0.069) H32(0.035) H34(0.044) H36(0.038) H37A(0.061)
 H37B(0.061) H37C(0.061) H38A(0.071) H38B(0.071) H38C(0.071) H40(0.036)
 H42(0.039) H44(0.033) H45A(0.065) H45B(0.065) H45C(0.065) H46A(0.055)
 H46B(0.055) H46C(0.055)
 Fixed X: H1A(0.8804) H1B(0.8654) H1C(0.8054) H2A(0.6917) H2B(0.7946)
 H2C(0.8129) H3A(0.6912) H3B(0.5946) H4A(0.5214) H4B(0.6226) H5A(0.5231)
 H5B(0.4122) H5C(0.4132) H6A(0.3581) H6B(0.3546) H6C(0.4278) H7A(0.9045)
 H7B(0.81) H8A(0.7936) H8B(0.9275) H9A(0.8996) H9B(0.8167) H10A(0.6578)
 H10B(0.7289) H11A(0.6147) H11B(0.5499) H12A(0.4597) H12B(0.3765) H13A(0.3377)
 H13B(0.4706) H14A(0.3578) H14B(0.4508) H47A(-0.0065) H47B(-0.0781) H48A(-
 0.1703) H48B(-0.2434) H48C(-0.1644) H48D(-0.2289) H50A(-0.2084) H50B(-0.131)
 H50C(-0.1322) H50D(-0.1817) H49A(-0.2872) H49B(-0.1671) H49C(-0.2935) H49D(-
 0.2737) H16(-0.0828) H18(-0.327) H20(0.0051) H21A(-0.2871) H21B(-0.3832) H21C(-
 0.3201) H22A(-0.2205) H22B(-0.1331) H22C(-0.262) H24(0.0336) H26(0.3111)
 H28(0.348) H29A(0.0062) H29B(0.1138) H29C(0.0751) H30A(0.5125) H30B(0.4925)
 H30C(0.513) H32(0.1404) H34(0.1147) H36(0.1262) H37A(0.1348) H37B(0.1649)
 H37C(0.0356) H38A(0.1833) H38B(0.057) H38C(0.0782) H40(0.3346) H42(0.3884)
 H44(0.0914) H45A(0.5455) H45B(0.5349) H45C(0.4908) H46A(0.1416) H46B(0.2535)
 H46C(0.1436)
 Fixed Y: H1A(0.2694) H1B(0.2324) H1C(0.3173) H2A(0.1039) H2B(0.1014)
 H2C(0.1404) H3A(0.1918) H3B(0.1561) H4A(0.2726) H4B(0.3287) H5A(0.4265)
 H5B(0.3929) H5C(0.4018) H6A(0.259) H6B(0.251) H6C(0.1875) H7A(0.3213)
 H7B(0.3907) H8A(0.3541) H8B(0.3391) H9A(0.1986) H9B(0.2156) H10A(0.2244)
 H10B(0.1568) H11A(0.4519) H11B(0.4794) H12A(0.5182) H12B(0.4875) H13A(0.3929)
 H13B(0.3845) H14A(0.3178) H14B(0.2719) H47A(0.5393) H47B(0.5785) H48A(0.4843)
 H48B(0.5445) H48C(0.5019) H48D(0.5157) H50A(0.7085) H50B(0.7124) H50C(0.6804)
 H50D(0.7324) H49A(0.6045) H49B(0.5784) H49C(0.6412) H49D(0.6084) H16(0.5045)
 H18(0.6223) H20(0.632) H21A(0.5413) H21B(0.5554) H21C(0.4686) H22A(0.7482)
 H22B(0.7007) H22C(0.6703) H24(0.4566) H26(0.3938) H28(0.5358) H29A(0.397)
 H29B(0.3729) H29C(0.3144) H30A(0.4169) H30B(0.4904) H30C(0.5101) H32(0.3694)
 H34(0.3204) H36(0.5574) H37A(0.2277) H37B(0.2067) H37C(0.2202) H38A(0.492)
 H38B(0.5224) H38C(0.4314) H40(0.5687) H42(0.8166) H44(0.7191) H45A(0.6442)
 H45B(0.7309) H45C(0.6491) H46A(0.8889) H46B(0.905) H46C(0.8657)
 Fixed Z: H1A(0.9518) H1B(1.0561) H1C(0.9994) H2A(0.8237) H2B(0.9493)
 H2C(0.848) H3A(1.0406) H3B(0.9236) H4A(0.9795) H4B(0.983) H5A(0.8444)
 H5B(0.8502) H5C(0.7304) H6A(0.6872) H6B(0.8059) H6C(0.7738) H7A(0.7779)
 H7B(0.7136) H8A(0.5377) H8B(0.6163) H9A(0.6356) H9B(0.5032) H10A(0.5321)
 H10B(0.6269) H11A(0.5871) H11B(0.6592) H12A(0.4482) H12B(0.4995) H13A(0.3502)
 H13B(0.3829) H14A(0.5075) H14B(0.4807) H47A(1.0792) H47B(0.9553) H48A(1.0556)
 H48B(0.9511) H48C(1.0907) H48D(0.9552) H50A(1.0302) H50B(1.1652) H50C(1.1788)
 H50D(1.0634) H49A(1.0848) H49B(1.1888) H49C(0.9717) H49D(1.0936) H16(0.5088)
 H18(0.5619) H20(0.8011) H21A(0.3426) H21B(0.3825) H21C(0.4035) H22A(0.7297)
 H22B(0.8411) H22C(0.7747) H24(0.8311) H26(1.1252) H28(0.8906) H29A(0.9883)
 H29B(1.1047) H29C(0.9964) H30A(1.1039) H30B(1.1731) H30C(1.0656) H32(0.7042)
 H34(0.39) H36(0.4951) H37A(0.6479) H37B(0.5467) H37C(0.5209) H38A(0.3195)
 H38B(0.286) H38C(0.2542) H40(0.7054) H42(0.7399) H44(0.7114) H45A(0.7976)
 H45B(0.7367) H45C(0.6624) H46A(0.6564) H46B(0.7727) H46C(0.7746)
;
_shelx_res_checksum              54630
_olex2_submission_special_instructions 'No special instructions were received'