Comproportionation of a dialuminyne with alane or dialane dihalides as a clean route to dialuminenes.
Queen, Joshua D.; Power, Philip P.; Chemical communications (Cambridge, England) 59 (2022) 43–46; doi:10.1039/d2cc05646a

data_7130969
_publ_section_title
;
 Comproportionation of a dialuminyne with alane or dialane dihalides as a
 clean route to dialuminenes.
;
_journal_issue                   1
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              43
_journal_page_last               46
_journal_paper_doi               10.1039/d2cc05646a
_journal_volume                  59
_journal_year                    2022
_chemical_formula_moiety         'C72 H96 Al2 Si2, 1.5(C6 H6)'
_chemical_formula_sum            'C81 H105 Al2 Si2'
_chemical_formula_weight         1188.78
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-10-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-10-11 deposited with the CCDC.	2022-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.426(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3894(11)
_cell_length_b                   19.669(2)
_cell_length_c                   32.660(6)
_cell_measurement_reflns_used    9366
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.60
_cell_measurement_theta_min      2.62
_cell_volume                     7314.2(17)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            43076
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.422
_diffrn_reflns_theta_min         1.209
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.7153
_exptl_absorpt_correction_T_min  0.6438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1032 before and 0.0425 after correction.
The Ratio of minimum to maximum transmission is 0.9000.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_description       block
_exptl_crystal_F_000             2580
_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.267
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.0108(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     789
_refine_ls_number_reflns         14960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+2.8137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13762
_reflns_number_total             14960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05646a2.cif
_cod_data_source_block           jq151fmi
_cod_depositor_comments
'Adding full bibliography for 7130967--7130970.cif.'
_cod_original_cell_volume        7314.1(16)
_cod_database_code               7130969
_shelx_shelxl_version_number     2014/7
_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.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28), C46(H46), C49(H49), C58(H58),
 C61(H61), C67(H67), C70(H70)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C21(H21), C22(H22), C23(H23),
 C36(H36), C38(H38), C42(H42), C43(H43), C44(H44), C54(H54), C55(H55), C56(H56),
  C68(H68), C69(H69), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75),
 C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C63(H63A,
 H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              16061
_shelx_hkl_checksum              70820
_olex2_submission_special_instructions 'No special instructions were received'