Chirality-Induced Catalyst Aggregation: Insights into Catalyst Speciation and Activity Using Chiral Aluminum Catalysts in Cyclic Ester Ring-Opening Polymerization
Gesslbauer, Sami; Hutchinson, George; White, Andrew J. P.; Burés, Jordi; Romain, Charles; ACS Catalysis 11 (2021) 4084–4093; doi:10.1021/acscatal.0c05245

data_4518561
_publ_section_title
;
 Chirality-Induced Catalyst Aggregation: Insights into Catalyst Speciation
 and Activity Using Chiral Aluminum Catalysts in Cyclic Ester Ring-Opening
 Polymerization
;
_journal_issue                   7
_journal_name_full               'ACS Catalysis'
_journal_page_first              4084
_journal_page_last               4093
_journal_paper_doi               10.1021/acscatal.0c05245
_journal_volume                  11
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C38 H61 Al N2 O3'
_chemical_formula_sum            'C38 H61 Al N2 O3'
_chemical_formula_weight         620.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 100.650(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.5311(3)
_cell_length_b                   12.1035(3)
_cell_length_c                   14.8941(4)
_cell_measurement_reflns_used    2166
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.5550
_cell_measurement_theta_min      4.2520
_cell_volume                     1865.75(9)
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.4115
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5815
_diffrn_reflns_point_group_measured_fraction_full 0.661
_diffrn_reflns_point_group_measured_fraction_max 0.630
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.224
_diffrn_reflns_theta_min         4.272
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       blocks
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.37(6)
_refine_ls_extinction_coef       0.00059(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         4705
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.5408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.267
_reflns_Friedel_fraction_full    0.306
_reflns_Friedel_fraction_max     0.280
_reflns_number_gt                4052
_reflns_number_total             4705
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c05245_si_002.cif
_cod_data_source_block           S_S-1
_cod_depositor_comments
'Adding full bibliography for 4518561--4518563.cif.'
_cod_original_cell_volume        1865.74(9)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4518561
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              57638
_shelx_hkl_checksum              99079