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_7131527
_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         'C42 H76 Al I N2 Si2'
_chemical_formula_sum            'C42 H76 Al I N2 Si2'
_chemical_formula_weight         819.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 112.8002(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8006(2)
_cell_length_b                   13.66544(13)
_cell_length_c                   18.6649(2)
_cell_measurement_reflns_used    16707
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5150
_cell_measurement_theta_min      4.7630
_cell_volume                     4420.66(9)
_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  (Sheldrick, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.993
_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  0.0379
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31520
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.682
_diffrn_reflns_theta_min         4.120
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.608
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35430
_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.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       plate
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.523
_refine_diff_density_min         -2.418
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         8869
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0696
_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^)+(0.1404P)^2^+11.7192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2034
_refine_ls_wR_factor_ref         0.2058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8446
_reflns_number_total             8869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01317k2.cif
_cod_data_source_block           ajrm067
_cod_depositor_comments
'Adding full bibliography for 7131527--7131531.cif.'
_cod_original_cell_volume        4420.64(10)
_cod_database_code               7131527
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.242
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13-C14 \\sim C13-C14A
 with sigma of 0.02
 C14-C13 \\sim C14A-C13
 with sigma of 0.005
 Al1-N2 \\sim Al2-N2
 with sigma of 0.005
 Al1-N1 \\sim Al2-N1
 with sigma of 0.005
 I1A-Al2 \\sim I1-Al1
 with sigma of 0.005
 Si2-C40 \\sim Si2-C40A
 with sigma of 0.005
 C41-C40 \\sim C42-C40 \\sim C42A-C40A \\sim C41A-C40A
 with sigma of 0.005
3. Restrained planarity
 N1, N2, I1A, Al2
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Al1 \\sim Al2: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.01 within 2A
C14 \\sim C14A: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.01 within 2A
I1 \\sim I1A: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01
within 2A
C40 \\sim C41 \\sim C42 \\sim C40A \\sim C41A \\sim C42A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.01 within 2A
Uanis(Al2) = Uanis(Al1)
5. Others
 Fixed Sof: H13(0.7) H13A(0.3) I1(0.96) Al1(0.96) C14(0.7) H14A(0.7) H14B(0.7)
 H14C(0.7) C40(0.7) H40(0.7) C41(0.7) H41A(0.7) H41B(0.7) H41C(0.7) C42(0.7)
 H42A(0.7) H42B(0.7) H42C(0.7) C14A(0.3) H14D(0.3) H14E(0.3) H14F(0.3)
 C40A(0.3) H40A(0.3) C41A(0.3) H41D(0.3) H41E(0.3) H41F(0.3) C42A(0.3)
 H42D(0.3) H42E(0.3) H42F(0.3) I1A(0.04) Al2(0.04)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C13(H13), C13(H13A), C16(H16), C28(H28), C31(H31), C34(H34),
  C37(H37), C19(H19), C40(H40), C40A(H40A)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C24(H24), C25(H25), C26(H26)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C14A(H14D,H14E,H14F), C41A(H41D,H41E,H41F),
 C42A(H42D,H42E,H42F)
;
_shelx_res_checksum              68984
_shelx_hkl_checksum              11695