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_7131531
_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_absolute_configuration unk
_chemical_formula_moiety         '0.5(C60 H104 Al2 K2 N4 Si4)'
_chemical_formula_sum            'C36 H58 Al K N2 Si2'
_chemical_formula_weight         641.10
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-07
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.1102(5)
_cell_length_b                   33.7684(8)
_cell_length_c                   10.7300(3)
_cell_measurement_reflns_used    21200
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      25.3320
_cell_measurement_theta_min      3.5940
_cell_volume                     8011.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            86594
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.042
_diffrn_reflns_theta_min         3.304
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.

Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- B-factor correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.063
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.41(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         14148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0578
_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^)+(0.0811P)^2^+3.6614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1595
_reflns_Friedel_coverage         0.815
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                13016
_reflns_number_total             14148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01317k2.cif
_cod_data_source_block           ajrm242
_cod_depositor_comments
'Adding full bibliography for 7131527--7131531.cif.'
_cod_database_code               7131531
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.923
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.59(7)
 0.41(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C25(H25), C28(H28), C7A(H7A), C10A(H10A), C25A(H25A),
 C28A(H28A)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C21(H21), C22(H22), C23(H23), C3A(H3A), C4A(H4A),
 C5A(H5A), C21A(H21A), C22A(H22A), C23A(H23A)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C8A(H8AA,H8AB,H8AC),
 C9A(H9AA,H9AB,H9AC), C11A(H11D,H11E,H11F), C12A(H12D,H12E,H12F), C13A(H13D,
 H13E,H13F), C14A(H14D,H14E,H14F), C15A(H15D,H15E,H15F), C16A(H16D,H16E,H16F),
 C17A(H17D,H17E,H17F), C18A(H18D,H18E,H18F), C26A(H26D,H26E,H26F), C27A(H27D,
 H27E,H27F), C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              57447
_shelx_hkl_checksum              24455