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_1557329
_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         'C36 H38 N4 O5 Al, C H2 Cl2'
_chemical_formula_sum            'C37 H40 Al Cl2 N4 O5'
_chemical_formula_weight         717.68
_chemical_name_common            '1:1 rac-LA:L7AlOBn'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                100.087(4)
_cell_angle_beta                 96.082(4)
_cell_angle_gamma                90.524(4)
_cell_formula_units_Z            2
_cell_length_a                   10.6552(10)
_cell_length_b                   12.4511(12)
_cell_length_c                   14.8269(16)
_cell_measurement_reflns_used    9284
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      2.25
_cell_volume                     1925.0(3)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX3, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'Shelxle-(Rev. 825) (Huebschle, C. B.,2011)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker PHOTON-II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38856
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.647
_diffrn_reflns_theta_min         2.253
_diffrn_source                   'micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       plate
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_exptl_transmission_factor_max   0.9813
_exptl_transmission_factor_min   0.9316
_refine_diff_density_max         0.981
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         10792
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+1.7934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8226
_reflns_number_total             10792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            L7AloLAOBn.cif.txt
_cod_data_source_block           final_a_sq
_cod_database_code               1557329
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.9102
_shelx_estimated_absorpt_t_max   0.9821
_shelx_res_checksum              99619
_shelx_hkl_checksum              79585
_shelx_fab_checksum              10593