An acyclic aluminyl anion.
Jackson, Ross A.; Matthews, Aidan J. R.; Vasko, Petra; Mahon, Mary F.; Hicks, Jamie; Liptrot, David J.; Chemical communications (Cambridge, England) 59 (2023) 5277–5280; doi:10.1039/d3cc01317k

data_7131528
_publ_section_title
;
 An acyclic aluminyl anion.
;
_journal_issue                   35
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5277
_journal_page_last               5280
_journal_paper_doi               10.1039/d3cc01317k
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C30 H52 Al I N2 Si2'
_chemical_formula_sum            'C30 H52 Al I N2 Si2'
_chemical_formula_weight         650.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-04
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-09 deposited with the CCDC.	2023-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                89.292(4)
_cell_angle_beta                 83.539(4)
_cell_angle_gamma                66.374(6)
_cell_formula_units_Z            2
_cell_length_a                   10.1072(6)
_cell_length_b                   10.2573(6)
_cell_length_c                   17.9608(8)
_cell_measurement_reflns_used    6323
_cell_measurement_temperature    149.9(7)
_cell_measurement_theta_max      29.7050
_cell_measurement_theta_min      3.6540
_cell_volume                     1694.04(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.9(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.852
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16043
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.279
_diffrn_reflns_theta_min         2.989
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_T_max  0.05167
_exptl_absorpt_correction_T_min  0.02647
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
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    1.276
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.101
_exptl_crystal_size_rad          0.079
_refine_diff_density_max         0.785
_refine_diff_density_min         -1.286
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         8652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0562P)^2^+1.8440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1280
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6769
_reflns_number_total             8652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01317k2.cif
_cod_data_source_block           e22djl07
_cod_depositor_comments
'Adding full bibliography for 7131527--7131531.cif.'
_cod_database_code               7131528
_shelxl_version_number           2014-3
_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. Uiso/Uaniso restraints and constraints
I1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
3.a Ternary CH refined with riding coordinates:
 C7(H7), C19(H19), C10(H10), C22(H22)
3.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C17(H17), C16(H16), C5(H5), C3(H3), C4(H4)
3.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C28(H28A,H28B,H28C), C20(H20A,H20B,H20C), C8(H8A,H8B,
 H8C), C25(H25A,H25B,H25C), C23(H23A,H23B,H23C), C21(H21A,H21B,H21C), C11(H11A,
 H11B,H11C), C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C9(H9A,H9B,H9C),
 C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              10104
_shelx_hkl_checksum              80827