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_7130967
_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         'C37 H55 Al I2 O Si'
_chemical_formula_sum            'C37 H55 Al I2 O Si'
_chemical_formula_weight         824.68
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_audit_creation_date             2022-08-07
_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                 97.410(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.998(2)
_cell_length_b                   13.500(3)
_cell_length_c                   26.336(5)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    90.15
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.17
_cell_volume                     3877.5(13)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      90.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0287
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            34107
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.466
_diffrn_reflns_theta_min         1.559
_diffrn_source_current           25.0
_diffrn_source_power             1.25
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.701
_exptl_absorpt_correction_T_max  0.7477
_exptl_absorpt_correction_T_min  0.6509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0562 before and 0.0333 after correction.
The Ratio of minimum to maximum transmission is 0.8705.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       Block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.076
_refine_diff_density_max         1.295
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         8898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+2.4074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0596
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7845
_reflns_number_total             8898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05646a2.cif
_cod_data_source_block           jq18fmi
_cod_depositor_comments
'Adding full bibliography for 7130967--7130970.cif.'
_cod_original_cell_volume        3877.6(13)
_cod_database_code               7130967
_shelx_shelxl_version_number     2014/7
_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.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C36(H36A,H36B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C21(H21), C22(H22), C23(H23)
2.d 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),
 C35(H35A,H35B,H35C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              79421
_shelx_hkl_checksum              17861
_olex2_submission_special_instructions 'No special instructions were received'