Mechanism of Initiation Stereocontrol in Polymerization of rac-Lactide by Aluminum Complexes Supported by Indolide‒Imine Ligands
Luke, Anna M.; Peterson, Appie; Chiniforoush, Sina; Mandal, Mukunda; Popowski, Yanay; Sajjad, Hussnain; Bouchey, Caitlin J.; Shopov, Dimitar Y.; Graziano, Brendan J.; Yao, Letitia J.; Cramer, Christopher J.; Reineke, Theresa M.; Tolman, William B.; Macromolecules  (2020) –; doi:10.1021/acs.macromol.0c00092

data_1557330
_publ_section_title
;
 Mechanism of Initiation Stereocontrol in Polymerization of rac-Lactide by
 Aluminum Complexes Supported by Indolide--Imine Ligands
;
_journal_name_full               Macromolecules
_journal_paper_doi               10.1021/acs.macromol.0c00092
_journal_year                    2020
_chemical_formula_moiety         'C30 H29 Al N4 O, 0.5(C7 H8)'
_chemical_formula_sum            'C33.5 H33 Al N4 O'
_chemical_formula_weight         534.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.827(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.393(2)
_cell_length_b                   20.309(4)
_cell_length_c                   11.565(2)
_cell_measurement_reflns_used    4365
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.747
_cell_measurement_theta_min      2.373
_cell_volume                     2813.9(9)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX 3, Bruker'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'area detector \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            36241
_diffrn_reflns_theta_full        25.38
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         1.97
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_recrystallization_method 'Chilled toluene solution'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5141
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+1.5800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1059
_reflns_number_gt                3665
_reflns_number_total             5141
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            L2AlOBn.cif.txt
_cod_data_source_block           wt50619-aap-1-116
_cod_original_formula_sum        'C33.50 H33 Al N4 O'
_cod_database_code               1557330
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C34-C33 \\sim C35-C34 \\sim C36-C35 \\sim C37-C36 \\sim C33-C32 \\sim C37-C32
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C36) = Uanis(C37) = Uanis(C32) = Uanis(C31) = Uanis(C33) = Uanis(C34) =
Uanis(C35)
4. Others
 Fixed Sof: C33(0.5) H33(0.5) C35(0.5) H35(0.5) C32(0.5) C34(0.5) H34(0.5)
 C36(0.5) H36(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) C37(0.5) H37(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C1(H1A,H1B), C21(H21A,H21B)
5.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C7(H7), C24(H24), C26(H26), C16(H16), C27(H27), C14(H14), C9(H9),
 C22(H22), C28(H28), C12(H12), C6(H6), C10(H10), C3(H3), C4(H4), C5(H5),
 C11(H11), C33(H33), C35(H35), C34(H34), C36(H36), C37(H37)
5.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C31(H31A,H31B,H31C)
;
_olex2_submission_original_sample_id AAP-1-116
_olex2_submission_special_instructions 'No special instructions were received'