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_7130968
_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         'C33 H45 Al I Si, C7 H8'
_chemical_formula_sum            'C40 H53 Al I Si'
_chemical_formula_weight         715.79
_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                 109.048(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4939(8)
_cell_length_b                   12.7921(7)
_cell_length_c                   18.3769(9)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    90.15
_cell_measurement_theta_max      72.29
_cell_measurement_theta_min      3.03
_cell_volume                     3887.3(3)
_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 0.987
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15859
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.291
_diffrn_reflns_theta_min         3.029
_diffrn_source_current           0.62
_diffrn_source_power             0.027745
_diffrn_source_voltage           44.75
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.154
_exptl_absorpt_correction_T_max  0.2732
_exptl_absorpt_correction_T_min  0.1443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0685 before and 0.0435 after correction.
The Ratio of minimum to maximum transmission is 0.5282.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       Block
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.121
_refine_diff_density_max         1.004
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         7423
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+7.6544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6871
_reflns_number_total             7423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05646a2.cif
_cod_data_source_block           jq27fmi
_cod_depositor_comments
'Adding full bibliography for 7130967--7130970.cif.'
_cod_database_code               7130968
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.478
_shelx_estimated_absorpt_t_min   0.316
_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
 C19-C20A
 1.43 with sigma of 0.02
3. Rigid bond restraints
 C34, C40
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C35 \\sim C36: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C38 \\sim C39: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C34 \\sim C40: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
5. Others
 Sof(C20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=
 Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27A)=
 Sof(H27D)=Sof(H27E)=Sof(H27F)=1-FVAR(1)
 Sof(C20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C25)=
 Sof(H25)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27A)=Sof(H27B)=
 Sof(H27C)=FVAR(1)
 Sof(I1A)=1-FVAR(2)
 Sof(I1)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28), C25A(H25A)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C21(H21), C22(H22), C23(H23),
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C21A(H21A), C22A(H22A),
 C23A(H23A)
6.c Fitted hexagon refined as free rotating group:
 C35(C36,C37,C38,C39,C34)
6.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),
 C40(H40A,H40B,H40C), C26A(H26D,H26E,H26F), C27A(H27D,H27E,H27F)
;
_shelx_res_checksum              15964
_shelx_hkl_checksum              92131
_olex2_submission_special_instructions 'No special instructions were received'