Extending Chain Growth Beyond C1 → C4 in CO Homologation: Aluminyl Promoted Formation of the [C5O5]5– Ligand
Evans, Matthew J.; Gardiner, Michael; Anker, Mathew David; Coles, Martyn P.; Chemical Communications  (2022) –; doi:10.1039/D2CC01554D

data_7129955
_publ_section_title
;
 Extending Chain Growth Beyond C1 \\rightarrow C4 in CO Homologation:
 Aluminyl Promoted Formation of the [C5O5]5-- Ligand
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01554D
_journal_year                    2022
_chemical_formula_moiety         'C60 H92 Al2 K2 N4 O6 Si4, C6 H14'
_chemical_formula_sum            'C66 H106 Al2 K2 N4 O6 Si4'
_chemical_formula_weight         1296.06
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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             2021-11-08T15:41:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2022-03-17 deposited with the CCDC.	2022-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.7646(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3863(2)
_cell_length_b                   13.1487(2)
_cell_length_c                   34.6062(4)
_cell_measurement_reflns_used    38289
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.218
_cell_measurement_theta_min      4.311
_cell_measurement_wavelength     1.54184
_cell_volume                     7404.29(17)
_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 0.9826
_diffrn_measured_fraction_theta_max 0.9922
_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      -0.072512
_diffrn_orient_matrix_UB_12      0.0486138
_diffrn_orient_matrix_UB_13      0.0178162
_diffrn_orient_matrix_UB_21      0.0458163
_diffrn_orient_matrix_UB_22      0.1025269
_diffrn_orient_matrix_UB_23      0.0032804
_diffrn_orient_matrix_UB_31      -0.0399376
_diffrn_orient_matrix_UB_32      0.0292219
_diffrn_orient_matrix_UB_33      -0.0410297
_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  0.0532
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            98397
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        74.0807
_diffrn_reflns_theta_max         73.6046
_diffrn_reflns_theta_min         3.514
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.359
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.389
_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            purple
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.342
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.109
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     760
_refine_ls_number_reflns         14834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0751P)^2^+3.7604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.135
_reflns_number_gt                13095
_reflns_number_total             14834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01554d2.cif
_cod_data_source_block           compound-1
_cod_original_cell_volume        7404.27(18)
_cod_database_code               7129955