Normal to abnormal I<sup>t</sup>Bu·AlH<sub>3</sub> isomerization in solution and in the solid state.
Chernysheva, Anna M.; Weinhart, Michael; Scheer, Manfred; Timoshkin, Alexey Y.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4665–4668; doi:10.1039/c9dt04698d

data_7703604
_publ_section_title
;
 Normal to abnormal I<sup>t</sup>Bu&#x00B7;AlH<sub>3</sub> isomerization
 in solution and in the solid state.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4665
_journal_page_last               4668
_journal_paper_doi               10.1039/c9dt04698d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C11 H23 Al N2'
_chemical_formula_sum            'C11 H23 Al N2'
_chemical_formula_weight         210.29
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-14
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.31 svn.r3677 for OlexSys, GUI svn.r5972)
;
_audit_update_record
;
2019-11-17 deposited with the CCDC.	2020-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.264(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5552(5)
_cell_length_b                   11.6275(7)
_cell_length_c                   13.9902(8)
_cell_measurement_reflns_used    4916
_cell_measurement_temperature    123.0(2)
_cell_measurement_theta_max      74.2000
_cell_measurement_theta_min      4.8880
_cell_volume                     1359.92(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -113.00 -20.00   1.00   10.00    --  -44.08 -57.00 -90.00   93
  2  \w   -130.00 -34.00   1.00   10.00    --  -44.08 178.00 -90.00   96
  3  \w     23.00 109.00   1.00   25.00    --  104.50 -94.00-150.00   86
  4  \w     36.00  98.00   1.00   25.00    --  104.50 -45.00 -60.00   62
  5  \w     33.00 121.00   1.00   25.00    --  104.50-125.00   0.00   88
  6  \w     79.00 174.00   1.00   25.00    --  104.50  61.00  30.00   95
  7  \w     27.00 141.00   1.00   25.00    --  104.50 -15.00   0.00  114
  8  \w   -116.00 -14.00   1.00   10.00    --  -44.08 -77.00  30.00  102
  9  \w   -116.00 -14.00   1.00   10.00    --  -44.08 -77.00 150.00  102
 10  \w     68.00 109.00   1.00   25.00    --  104.50  15.00-180.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0207521000
_diffrn_orient_matrix_UB_12      -0.1001182000
_diffrn_orient_matrix_UB_13      0.0737017000
_diffrn_orient_matrix_UB_21      0.0757186000
_diffrn_orient_matrix_UB_22      0.0829822000
_diffrn_orient_matrix_UB_23      0.0828383000
_diffrn_orient_matrix_UB_31      -0.1668229000
_diffrn_orient_matrix_UB_32      0.0252223000
_diffrn_orient_matrix_UB_33      0.0202183000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7331
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.701
_diffrn_reflns_theta_min         4.993
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.533
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.027
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.131
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0055(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2672
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0599
_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^)+(0.1094P)^2^+0.3579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1670
_refine_ls_wR_factor_ref         0.1755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2368
_reflns_number_total             2672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04698d2.cif
_cod_data_source_block           mw141_mp_abs_gaus
_cod_depositor_comments
'Adding full bibliography for 7703603--7703604.cif.'
_cod_database_code               7703604
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C11H23AlN2
_chemical_oxdiff_usercomment     'clear blocks'
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.649
_reflns_odcompleteness_completeness 99.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C),
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              24719
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.658
_oxdiff_exptl_absorpt_empirical_full_min 0.284