Ring-Expansion and Desulfurisation of Thiophenes with an Aluminium(I) Reagent
McMullen, Jacob; White, Andrew J. P.; Crimmin, Mark Richard; Chemical Communications  (2023) –; doi:10.1039/D3CC04594C

data_7132353
_publ_section_title
;
 Ring-Expansion and Desulfurisation of Thiophenes with an Aluminium(I)
 Reagent
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC04594C
_journal_year                    2023
_chemical_formula_moiety         'C34 H47 Al N2 S, C7 H8'
_chemical_formula_sum            'C41 H55 Al N2 S'
_chemical_formula_weight         634.91
_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_method           SHELXL-2018/3
_audit_update_record
;
2023-09-05 deposited with the CCDC.	2023-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                104.737(3)
_cell_angle_beta                 90.087(3)
_cell_angle_gamma                97.200(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4074(4)
_cell_length_b                   10.9429(4)
_cell_length_c                   17.0594(6)
_cell_measurement_reflns_used    7611
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.4050
_cell_measurement_theta_min      4.2030
_cell_volume                     1862.99(12)
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.4115
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31624
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.949
_diffrn_reflns_theta_min         4.213
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.209
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_description       blocks
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.278
_exptl_crystal_size_min          0.194
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         7418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0650
_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^)+(0.0991P)^2^+1.4540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1728
_refine_ls_wR_factor_ref         0.1973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5452
_reflns_number_total             7418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04594c3.cif
_cod_data_source_block           2b
_cod_database_code               7132353
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              49813
_shelx_hkl_checksum              71411