Aluminyl derived ethene functionalization with heteroallenes, leading to an intramolecular ligand rearrangement.
O'Reilly, Andrea; Gardiner, Michael G.; McMullin, Claire L.; Fulton, J. Robin; Coles, Martyn P.; Chemical communications (Cambridge, England) 60 (2024) 881–884; doi:10.1039/d3cc05785b

data_7132540
_publ_section_title
;
 Aluminyl derived ethene functionalization with heteroallenes, leading to
 an intramolecular ligand rearrangement.
;
_journal_issue                   7
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              881
_journal_page_last               884
_journal_paper_doi               10.1039/d3cc05785b
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C74 H128 Al2 K2 N8 O2 Si4, 7(C6 H6)'
_chemical_formula_sum            'C116 H170 Al2 K2 N8 O2 Si4'
_chemical_formula_weight         1953.11
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2022-07-25T16:44:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2023-11-26 deposited with the CCDC.	2023-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.1459(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
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_cell_length_b                   23.22737(19)
_cell_length_c                   19.4534(2)
_cell_measurement_reflns_used    24731
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      73.437
_cell_measurement_theta_min      4.015
_cell_measurement_wavelength     1.54184
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_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.9943
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1060993
_diffrn_orient_matrix_UB_12      0.0146618
_diffrn_orient_matrix_UB_13      -0.0560864
_diffrn_orient_matrix_UB_21      0.0560072
_diffrn_orient_matrix_UB_22      0.0153502
_diffrn_orient_matrix_UB_23      -0.0556297
_diffrn_orient_matrix_UB_31      -0.0111199
_diffrn_orient_matrix_UB_32      -0.0628317
_diffrn_orient_matrix_UB_33      -0.0265739
_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  0.0301
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49574
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        74.0807
_diffrn_reflns_theta_max         73.591
_diffrn_reflns_theta_min         3.5379
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.65
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.508
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
                        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2116
_exptl_crystal_size_max          0.329
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.227
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     636
_refine_ls_number_reflns         11593
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+2.2896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1
_reflns_number_gt                10469
_reflns_number_total             11593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05785b2.cif
_cod_data_source_block           Compound-3-C6H6
_cod_depositor_comments
'Adding full bibliography for 7132539--7132541.cif.'
_cod_original_cell_volume        5777.77(11)
_cod_database_code               7132540