Controlled reductive C-C coupling of isocyanides promoted by an aluminyl anion.
Evans, Matthew J.; Anker, Mathew D.; McMullin, Claire L.; Coles, Martyn P.; Chemical science 14 (2023) 6278–6288; doi:10.1039/d3sc01387a

data_1569174
_publ_section_title
;
 Controlled reductive C-C coupling of isocyanides promoted by an aluminyl
 anion.
;
_journal_issue                   23
_journal_name_full               'Chemical science'
_journal_page_first              6278
_journal_page_last               6288
_journal_paper_doi               10.1039/d3sc01387a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         '2(C55 H73 Al K N5 O Si2), 3(C7 H8)'
_chemical_formula_sum            'C131 H170 Al2 K2 N10 O2 Si4'
_chemical_formula_weight         2161.28
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_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             2021-07-28T14:56:34-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2023-03-09 deposited with the CCDC.	2023-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                82.310(2)
_cell_angle_beta                 76.873(2)
_cell_angle_gamma                80.547(2)
_cell_formula_units_Z            1
_cell_length_a                   11.0552(3)
_cell_length_b                   11.8345(3)
_cell_length_c                   23.9671(7)
_cell_measurement_reflns_used    11100
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.124
_cell_measurement_theta_min      4.067
_cell_measurement_wavelength     1.54184
_cell_volume                     2997.03(14)
_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      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_measured_fraction_theta_full 0.9752
_diffrn_measured_fraction_theta_max 0.9925
_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      -0.0433513
_diffrn_orient_matrix_UB_12      -0.1158176
_diffrn_orient_matrix_UB_13      -0.0031148
_diffrn_orient_matrix_UB_21      0.0692778
_diffrn_orient_matrix_UB_22      0.0003501
_diffrn_orient_matrix_UB_23      -0.0635093
_diffrn_orient_matrix_UB_31      0.119154
_diffrn_orient_matrix_UB_32      -0.0646462
_diffrn_orient_matrix_UB_33      0.0189122
_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  0.0478
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            39077
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        74.3338
_diffrn_reflns_theta_max         73.3034
_diffrn_reflns_theta_min         3.8058
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.646
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.745
_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            'dark purple'
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1162
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     725
_refine_ls_number_reflns         11958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0903
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0775P)^2^+11.8819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2267
_refine_ls_wR_factor_ref         0.2336
_reflns_number_gt                10186
_reflns_number_total             11958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01387a2.cif
_cod_data_source_block           compound-2-toluene
_cod_depositor_comments
'Adding full bibliography for 1569168--1569174.cif.'
_cod_original_cell_volume        2997.04(14)
_cod_database_code               1569174