Synthesis and reactivity of a terminal aluminium-imide bond.
Anker, Mathew D.; Schwamm, Ryan J.; Coles, Martyn P.; Chemical communications (Cambridge, England) 56 (2020) 2288–2291; doi:10.1039/c9cc09214e

data_7125829
_publ_section_title
;
 Synthesis and reactivity of a terminal aluminium-imide bond.
;
_journal_issue                   15
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2288
_journal_page_last               2291
_journal_paper_doi               10.1039/c9cc09214e
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C74 H114 Al2 K2 N6 O2 Si4, 2(C6 H14)'
_chemical_formula_sum            'C86 H142 Al2 K2 N6 O2 Si4'
_chemical_formula_weight         1536.58
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2018-07-06T11:05:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-11-25 deposited with the CCDC.	2020-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.7014(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.00568(11)
_cell_length_b                   19.41913(17)
_cell_length_c                   19.00129(17)
_cell_measurement_reflns_used    18864
_cell_measurement_temperature    119.94(16)
_cell_measurement_theta_max      73.481
_cell_measurement_theta_min      4.336
_cell_measurement_wavelength     1.54184
_cell_volume                     4619.87(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      119.94(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0292281
_diffrn_orient_matrix_UB_12      0.0560635
_diffrn_orient_matrix_UB_13      -0.0594548
_diffrn_orient_matrix_UB_21      -0.0340919
_diffrn_orient_matrix_UB_22      0.048267
_diffrn_orient_matrix_UB_23      0.0540355
_diffrn_orient_matrix_UB_31      0.1145043
_diffrn_orient_matrix_UB_32      0.0286254
_diffrn_orient_matrix_UB_33      0.0253995
_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  0.0279
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35415
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        68.1328
_diffrn_reflns_theta_max         68.2507
_diffrn_reflns_theta_min         3.6993
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.931
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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_density_diffrn    1.105
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     477
_refine_ls_number_reflns         8467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.034
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+1.4261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                7718
_reflns_number_total             8467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09214e2.cif
_cod_data_source_block           Compound-1
_cod_depositor_comments
'Adding full bibliography for 7125829--7125830.cif.'
_cod_original_sg_symbol_H-M      'P 2/n '
_cod_database_code               7125829