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_7131529
_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         'C59 H93 Al Mg N4 Si2, C7 H8'
_chemical_formula_sum            'C66 H101 Al Mg N4 Si2'
_chemical_formula_weight         1057.97
_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             2022-08-09
_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                87.531(3)
_cell_angle_beta                 83.372(3)
_cell_angle_gamma                84.087(3)
_cell_formula_units_Z            2
_cell_length_a                   12.8772(5)
_cell_length_b                   14.6377(6)
_cell_length_c                   17.2412(6)
_cell_measurement_reflns_used    14377
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.4410
_cell_measurement_theta_min      4.3830
_cell_volume                     3209.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_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           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23418
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.639
_diffrn_reflns_theta_min         3.472
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.095
_exptl_crystal_description       block
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.157
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         12477
_refine_ls_number_restraints     217
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0698P)^2^+1.2118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1224
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11296
_reflns_number_total             12477
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01317k2.cif
_cod_data_source_block           s22djl17
_cod_depositor_comments
'Adding full bibliography for 7131527--7131531.cif.'
_cod_database_code               7131529
_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. Restrained distances
 C66-C60 \\sim C66A-C60A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C60A
\\sim C61A \\sim C62A \\sim C63A \\sim C64A \\sim C65A \\sim C66A: within 2A
with sigma of 0.015 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Fixed Sof: C60(0.5) C61(0.5) H64(0.5) C62(0.5) H63(0.5) C63(0.5) H62(0.5)
 C64(0.5) H61(0.5) C65(0.5) H60(0.5) C66(0.5) H65A(0.5) H65B(0.5) H65C(0.5)
 C60A(0.5) C61A(0.5) H64A(0.5) C62A(0.5) H63A(0.5) C63A(0.5) H62A(0.5)
 C64A(0.5) H61A(0.5) C65A(0.5) H60A(0.5) C66A(0.5) H65D(0.5) H65E(0.5) H65F(0.5)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C22(H22), C25(H25), C42(H41), C45(H44), C54(H56), C57(H53)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C18(H18), C19(H19), C20(H20), C33(H32), C38(H36),
 C39(H37), C40(H38), C50(H51), C51(H50), C52(H49), C61(H64), C62(H63), C63(H62),
  C64(H61), C65(H60), C61A(H64A), C62A(H63A), C63A(H62A), C64A(H61A), C65A(H60A)
5.c Fitted hexagon refined as free rotating group:
 C60(C61,C62,C63,C64,C65), C60A(C61A,C62A,C63A,C64A,C65A)
5.d 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), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H01A,H01B,H01C),
 C35(H01D,H01E,H01F), C43(H42A,H42B,H42C), C44(H43A,H43B,H43C), C46(H45A,H45B,
 H45C), C47(H46A,H46B,H46C), C55(H58A,H58B,H58C), C56(H57A,H57B,H57C), C59(H55A,
 H55B,H55C), C58(H54B,H54A,H54C), C66(H65A,H65B,H65C), C66A(H65D,H65E,H65F)
;
_shelx_res_checksum              39172
_shelx_hkl_checksum              83592