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_7130599
_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         'C51 H75 Al Mg N4 O2 Si2, 2(C7 H8)'
_chemical_formula_sum            'C65 H91 Al Mg N4 O2 Si2'
_chemical_formula_weight         1067.88
_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             2022-03-10T15:23:27-00:00
_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                 96.081(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.0112(4)
_cell_length_b                   26.6902(5)
_cell_length_c                   26.0942(6)
_cell_measurement_reflns_used    19645
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.291
_cell_measurement_theta_min      4.041
_cell_measurement_wavelength     1.54184
_cell_volume                     13166.0(5)
_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 0.9776
_diffrn_measured_fraction_theta_max 0.9884
_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      -0.0744866
_diffrn_orient_matrix_UB_12      -0.0233487
_diffrn_orient_matrix_UB_13      -0.0069833
_diffrn_orient_matrix_UB_21      -0.0035656
_diffrn_orient_matrix_UB_22      0.0086385
_diffrn_orient_matrix_UB_23      -0.0586206
_diffrn_orient_matrix_UB_31      0.0328387
_diffrn_orient_matrix_UB_32      -0.0520541
_diffrn_orient_matrix_UB_33      -0.0065791
_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  0.0427
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            87564
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        74.0807
_diffrn_reflns_theta_max         73.4317
_diffrn_reflns_theta_min         3.4573
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.445
_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    1.078
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4624
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1139
_refine_ls_number_reflns         26221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0679
_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^)+(0.1121P)^2^+9.0123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1931
_refine_ls_wR_factor_ref         0.211
_reflns_number_gt                18454
_reflns_number_total             26221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04028j2.cif
_cod_data_source_block           Compound-4-Mg
_cod_depositor_comments
;

2024-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C130 H182 Al2 Mg2 N8 O4 Si4'
_cod_original_formula_weight         2135.77
_cod_original_formula_moiety         '2(C51 H75 Al Mg N4 O2 Si2), 4(C7 H8)'
_cod_original_formula_units_Z            4
_cod_database_code               7130599