NHI- and NHC-Supported Al(III) Hydrides for Amine-Borane Dehydrocoupling Catalysis
Weetman, C.; Ito, N.; Unno, M.; Hanusch, F.; Inoue, S.; Inorganics 7 (2019) 92–; doi:10.3390/inorganics7080092

data_1556418
_publ_section_title
;
 NHI- and NHC-Supported Al(III) Hydrides for Amine-Borane Dehydrocoupling
 Catalysis
;
_journal_name_full               Inorganics
_journal_page_first              92
_journal_paper_doi               10.3390/inorganics7080092
_journal_volume                  7
_journal_year                    2019
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C31 H55 Al B2 N4'
_chemical_formula_sum            'C31 H55 Al B2 N4'
_chemical_formula_weight         532.39
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 104.73(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.135(9)
_cell_length_b                   18.687(14)
_cell_length_c                   19.155(15)
_cell_measurement_reflns_used    8820
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.1718
_cell_measurement_theta_min      2.1678
_cell_volume                     3509(5)
_computing_cell_refinement       'SAINT (Bruker, 2017)'
_computing_data_collection       'APEX III Control Software (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2017)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'
_computing_structure_refinement
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 ' CMOS plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker Photon CMOS '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  'Helios optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'TXS rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1316
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            87849
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.62
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.735
_exptl_absorpt_correction_T_min  0.662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2, Bruker, 2016'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.008
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.252
_exptl_crystal_size_min          0.178
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_Flack   .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6558
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[\S^2^(FO^2^)+(0.0494P)^2^+1.8193P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1319
_reflns_number_gt                4722
_reflns_number_total             6558
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            Inorganics-2019-7-92.cif
_cod_data_source_block           itono1_fine
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1556418
_shelx_res_checksum              80711
_shelx_hkl_checksum              9880