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_7130970
_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         '0.5(C66 H90 Al2 Na2 Si2), 1.5(C7 H8)'
_chemical_formula_sum            'C43.5 H57 Al Na Si'
_chemical_formula_weight         657.95
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_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                98.4810(10)
_cell_angle_beta                 90.4220(10)
_cell_angle_gamma                106.9270(10)
_cell_formula_units_Z            4
_cell_length_a                   11.4744(10)
_cell_length_b                   17.7494(15)
_cell_length_c                   21.1607(18)
_cell_measurement_reflns_used    9840
_cell_measurement_temperature    90.15
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.78
_cell_volume                     4072.1(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0203
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37051
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_min         1.671
_diffrn_source_current           25.0
_diffrn_source_power             1.25
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0445 before and 0.0325 after correction.
The Ratio of minimum to maximum transmission is 0.8645.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.073
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.629
_exptl_crystal_size_mid          0.326
_exptl_crystal_size_min          0.282
_refine_diff_density_max         1.299
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     982
_refine_ls_number_reflns         18661
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0812P)^2^+1.7856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1480
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14882
_reflns_number_total             18661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05646a2.cif
_cod_data_source_block           jq20fmi
_cod_depositor_comments
'Adding full bibliography for 7130967--7130970.cif.'
_cod_original_formula_sum        'C43.50 H57 Al Na Si'
_cod_database_code               7130970
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.930
_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
 C71-C77 = C71B-C77B = C81-C87
 1.5 with sigma of 0.01
 C101-C107
 1.5 with sigma of 0.01
 C91-C97 = C91B-C97B
 1.5 with sigma of 0.01
 C102-C107 \\sim C106-C107
 with sigma of 0.01
 C72-C77 \\sim C76-C77 \\sim C72B-C77B \\sim C76B-C77B \\sim C82-C87 \\sim
C86-C87
 with sigma of 0.01
 C92-C97 \\sim C96-C97 \\sim C92B-C97B \\sim C96B-C97B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C92 \\sim C92B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
4. Others
 Fixed Sof: C71(0.5) C72(0.5) H72(0.5) C73(0.5) H73(0.5) C74(0.5) H74(0.5)
 C75(0.5) H75(0.5) C76(0.5) H76(0.5) C77(0.5) H77A(0.5) H77B(0.5) H77C(0.5)
 C71B(0.5) C72B(0.5) H72B(0.5) C73B(0.5) H73B(0.5) C74B(0.5) H74B(0.5)
 C75B(0.5) H75B(0.5) C76B(0.5) H76B(0.5) C77B(0.5) H77D(0.5) H77E(0.5)
 H77F(0.5) C81(0.5) C82(0.5) H82(0.5) C83(0.5) H83(0.5) C84(0.5) H84(0.5)
 C85(0.5) H85(0.5) C86(0.5) H86(0.5) C87(0.5) H87A(0.5) H87B(0.5) H87C(0.5)
 C91(0.81) C92(0.81) H92(0.81) C93(0.81) H93(0.81) C94(0.81) H94(0.81)
 C95(0.81) H95(0.81) C96(0.81) H96(0.81) C97(0.81) H97A(0.81) H97B(0.81)
 H97C(0.81) C91B(0.19) C92B(0.19) H92B(0.19) C93B(0.19) H93B(0.19) C94B(0.19)
 H94B(0.19) C95B(0.19) H95B(0.19) C96B(0.19) H96B(0.19) C97B(0.19) H97D(0.19)
 H97E(0.19) H97F(0.19) C101(0.5) C102(0.5) H102(0.5) C103(0.5) H103(0.5)
 C104(0.5) H104(0.5) C105(0.5) H105(0.5) C106(0.5) H106(0.5) C107(0.5)
 H10A(0.5) H10B(0.5) H10C(0.5)
5.a Ternary CH refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C13(H13), C16(H16), C21(H21), C22(H22), C23(H23),
 C25(H25), C28(H28), C42(H42), C43(H43), C44(H44), C46(H46), C49(H49), C54(H54),
  C55(H55), C56(H56), C58(H58), C61(H61)
5.b Me refined with riding coordinates:
 C87(H87A,H87B,H87C)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C36(H36), C38(H38), C72(H72), C73(H73), C74(H74), C75(H75),
 C76(H76), C72B(H72B), C73B(H73B), C74B(H74B), C75B(H75B), C76B(H76B), C82(H82),
  C83(H83), C84(H84), C85(H85), C86(H86), C92(H92), C93(H93), C94(H94),
 C95(H95), C96(H96), C92B(H92B), C93B(H93B), C94B(H94B), C95B(H95B), C96B(H96B),
  C102(H102), C103(H103), C104(H104), C105(H105), C106(H106)
5.d Fitted hexagon refined as free rotating group:
 C71(C72,C73,C74,C75,C76), C71B(C72B,C73B,C74B,C75B,C76B), C81(C82,C83,C84,C85,
 C86), C91(C92,C93,C94,C95,C96), C91B(C92B,C93B,C94B,C95B,C96B), C101(C102,C103,
 C104,C105,C106)
5.e 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),
 C77(H77A,H77B,H77C), C77B(H77D,H77E,H77F), C97(H97A,H97B,H97C), C97B(H97D,H97E,
 H97F), C107(H10A,H10B,H10C)
;
_shelx_res_checksum              79517
_shelx_hkl_checksum              90629
_olex2_submission_special_instructions 'No special instructions were received'