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_1569170
_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         'C67 H101.61 Al K N5 O3 Si2'
_chemical_formula_sum            'C67 H101.61 Al K N5 O3 Si2'
_chemical_formula_weight         1147.4
_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             2021-10-29T14:20:03-00:00
_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                84.046(4)
_cell_angle_beta                 88.135(4)
_cell_angle_gamma                65.381(5)
_cell_formula_units_Z            2
_cell_length_a                   12.7748(6)
_cell_length_b                   14.6769(7)
_cell_length_c                   19.1675(8)
_cell_measurement_reflns_used    9093
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.935
_cell_measurement_theta_min      3.866
_cell_measurement_wavelength     1.54184
_cell_volume                     3249.3(3)
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_measured_fraction_theta_full 0.9783
_diffrn_measured_fraction_theta_max 0.9936
_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      0.0618079
_diffrn_orient_matrix_UB_12      0.0628207
_diffrn_orient_matrix_UB_13      -0.0352825
_diffrn_orient_matrix_UB_21      0.1159464
_diffrn_orient_matrix_UB_22      -0.0932162
_diffrn_orient_matrix_UB_23      0.0084974
_diffrn_orient_matrix_UB_31      -0.0183073
_diffrn_orient_matrix_UB_32      -0.0287774
_diffrn_orient_matrix_UB_33      -0.0722083
_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  0.0424
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43228
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        74.0807
_diffrn_reflns_theta_max         73.2383
_diffrn_reflns_theta_min         3.8064
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.564
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.802
_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            red
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1245.22
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     864
_refine_ls_number_reflns         12963
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+1.6957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1426
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                10297
_reflns_number_total             12963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01387a2.cif
_cod_data_source_block           compound-4-THF
_cod_depositor_comments
'Adding full bibliography for 1569168--1569174.cif.'
_cod_database_code               1569170