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_7703603
_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      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.99950(10)
_cell_length_b                   13.99950(10)
_cell_length_c                   13.7306(2)
_cell_measurement_reflns_used    5918
_cell_measurement_temperature    122.98(10)
_cell_measurement_theta_max      73.3560
_cell_measurement_theta_min      4.4810
_cell_volume                     2691.01(5)
_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      122.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.959
_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   -116.00 -22.00   1.00    1.00    --  -44.92 -37.00  30.00   94
  2  \w     32.00  91.00   1.00    5.00    --  104.50 -30.00  30.00   59
  3  \w     36.00  98.00   1.00    5.00    --  104.50 -45.00  90.00   62
  4  \w     35.00 130.00   1.00    5.00    --  104.50 -61.00 -90.00   95
  5  \w   -113.00 -88.00   1.00    1.00    --  -44.92 -57.00 150.00   25
  6  \w   -117.00 -15.00   1.00    1.00    --  -44.92 -77.00 -90.00  102
;
_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      -0.1034761000
_diffrn_orient_matrix_UB_12      -0.0092454000
_diffrn_orient_matrix_UB_13      -0.0369521000
_diffrn_orient_matrix_UB_21      -0.0101099000
_diffrn_orient_matrix_UB_22      0.1095954000
_diffrn_orient_matrix_UB_23      0.0010520000
_diffrn_orient_matrix_UB_31      0.0360123000
_diffrn_orient_matrix_UB_32      0.0042776000
_diffrn_orient_matrix_UB_33      -0.1059253000
_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  0.0187
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7413
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.444
_diffrn_reflns_theta_min         4.467
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.061
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.396
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.952
_exptl_crystal_size_mid          0.355
_exptl_crystal_size_min          0.287
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       0.0023(2)
_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   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0473P)^2^+0.8015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2504
_reflns_number_total             2605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04698d2.cif
_cod_data_source_block           mw329_tp_abs_gaus
_cod_depositor_comments
'Adding full bibliography for 7703603--7703604.cif.'
_cod_original_cell_volume        2691.00(5)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               7703603
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C11H23AlN2
_shelx_estimated_absorpt_t_max   0.750
_shelx_estimated_absorpt_t_min   0.431
_reflns_odcompleteness_completeness 98.93
_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:
 C3(H3), C2(H2)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C),
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              87301
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.670
_oxdiff_exptl_absorpt_empirical_full_min 0.790