Isolating elusive ‘Al(μ-O)M’ intermediates in CO2 reduction by bimetallic Al–M complexes (M = Zn, Mg)
Evans, Matthew J.; Iliffe, George H.; Neale, Samuel E.; McMullin, Claire L.; Fulton, J. Robin; Anker, Mathew D.; Coles, Martyn P.; Chemical Communications  (2022) –; doi:10.1039/D2CC04028J

data_7130598
_publ_section_title
;
 Isolating elusive &#x2018;Al(\m-O)M&#x2019; intermediates in CO2
 reduction by bimetallic Al--M complexes (M = Zn, Mg)
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04028J
_journal_year                    2022
_chemical_formula_moiety         'C52 H75 Al N4 O4 Si2 Zn'
_chemical_formula_sum            'C52 H75 Al N4 O4 Si2 Zn'
_chemical_formula_weight         968.69
_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             2021-12-16T10:58:54-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2022-07-04 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.8850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.56239(17)
_cell_length_b                   15.0196(2)
_cell_length_c                   25.1167(3)
_cell_measurement_reflns_used    16204
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.89
_cell_measurement_theta_min      4.252
_cell_measurement_wavelength     1.54184
_cell_volume                     5441.62(12)
_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 0.9789
_diffrn_measured_fraction_theta_max 0.9931
_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      0.0808466
_diffrn_orient_matrix_UB_12      0.0420012
_diffrn_orient_matrix_UB_13      -0.0247763
_diffrn_orient_matrix_UB_21      -0.0628126
_diffrn_orient_matrix_UB_22      0.0786673
_diffrn_orient_matrix_UB_23      -0.0208389
_diffrn_orient_matrix_UB_31      0.0303134
_diffrn_orient_matrix_UB_32      0.0506904
_diffrn_orient_matrix_UB_33      0.0527962
_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  0.0267
_diffrn_reflns_av_unetI/netI     0.042
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40320
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        74.0807
_diffrn_reflns_theta_max         73.24
_diffrn_reflns_theta_min         3.747
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.55
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.462
_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            colourless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     597
_refine_ls_number_reflns         10851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.041
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0486P)^2^+2.1406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                9420
_reflns_number_total             10851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04028j2.cif
_cod_data_source_block           Compound-5
_cod_original_cell_volume        5441.60(11)
_cod_database_code               7130598