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_7129957
_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
'C128 H200 Al4 K6 N10 O14 Si8, 2(C7 H8), 2.5 (C6 H16 N2)'
_chemical_formula_sum            'C157 H256 Al4 K6 N15 O14 Si8'
_chemical_formula_weight         3144.99
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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             2021-10-23T15:43:56-00:00
_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                 97.0291(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.48560(7)
_cell_length_b                   32.8594(2)
_cell_length_c                   36.3809(2)
_cell_measurement_reflns_used    49335
_cell_measurement_temperature    150(3)
_cell_measurement_theta_max      73.152
_cell_measurement_theta_min      4.207
_cell_measurement_wavelength     1.54184
_cell_volume                     18373.19(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(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_measured_fraction_theta_full 0.9793
_diffrn_measured_fraction_theta_max 0.99
_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      0.004903
_diffrn_orient_matrix_UB_12      0.0250332
_diffrn_orient_matrix_UB_13      0.0360099
_diffrn_orient_matrix_UB_21      -0.0045501
_diffrn_orient_matrix_UB_22      0.0396361
_diffrn_orient_matrix_UB_23      -0.0227731
_diffrn_orient_matrix_UB_31      -0.0999876
_diffrn_orient_matrix_UB_32      -0.0005772
_diffrn_orient_matrix_UB_33      -0.0024098
_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  0.0313
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.99
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            148511
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.99
_diffrn_reflns_theta_full        73.8322
_diffrn_reflns_theta_max         73.3035
_diffrn_reflns_theta_min         3.5269
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.398
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.607
_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    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6772
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.119
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.01
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1613
_refine_ls_number_reflns         36547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.01
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0663P)^2^+10.2785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1292
_reflns_number_gt                31728
_reflns_number_total             36547
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01554d2.cif
_cod_data_source_block           compound-2
_cod_original_cell_volume        18373.18(19)
_cod_database_code               7129957