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_1569173
_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_absolute_configuration ad
_chemical_formula_moiety         'C61 H91 Al K N5 O Si2, C7 H8'
_chemical_formula_sum            'C68 H99 Al K N5 O Si2'
_chemical_formula_weight         1124.78
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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             2021-11-25T13:00:39-00:00
_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                90
_cell_angle_beta                 136.513(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   36.4496(7)
_cell_length_b                   12.44536(9)
_cell_length_c                   20.2703(4)
_cell_measurement_reflns_used    14004
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.161
_cell_measurement_theta_min      4.489
_cell_measurement_wavelength     1.54184
_cell_volume                     6328.0(4)
_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 0.9767
_diffrn_measured_fraction_theta_max 0.6296
_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      0.0440675
_diffrn_orient_matrix_UB_12      0.0860232
_diffrn_orient_matrix_UB_13      0.0535898
_diffrn_orient_matrix_UB_21      0.0420333
_diffrn_orient_matrix_UB_22      -0.0888023
_diffrn_orient_matrix_UB_23      0.0445895
_diffrn_orient_matrix_UB_31      -0.0079556
_diffrn_orient_matrix_UB_32      0.007489
_diffrn_orient_matrix_UB_33      -0.0855375
_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  0.0255
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20829
_diffrn_reflns_point_group_measured_fraction_full 0.644
_diffrn_reflns_point_group_measured_fraction_max 0.633
_diffrn_reflns_theta_full        73.8322
_diffrn_reflns_theta_max         73.29
_diffrn_reflns_theta_min         3.524
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.575
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.754
_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            'pale yellow'
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Flack x determined using 1672 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     716
_refine_ls_number_reflns         8059
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0355P)^2^+1.7151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0606
_reflns_number_gt                7878
_reflns_number_total             8059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01387a2.cif
_cod_data_source_block           compound-5-toluene
_cod_depositor_comments
'Adding full bibliography for 1569168--1569174.cif.'
_cod_original_cell_volume        6328.05(18)
_cod_database_code               1569173