Highly Active Chiral Oxazolinyl Aminophenolate Magnesium Initiators for Isoselective Ring-Opening Polymerization of rac-Lactide: Dinuclearity Induced Enantiomorphic Site Control
Hu, Jianwen; Kan, Chao; Wang, Haobing; Ma, Haiyan; Macromolecules 51 (2018) 5304–; doi:10.1021/acs.macromol.8b00924

data_1552828
_publ_section_title
;
 Highly Active Chiral Oxazolinyl Aminophenolate Magnesium Initiators for
 Isoselective Ring-Opening Polymerization of rac-Lactide: Dinuclearity
 Induced Enantiomorphic Site Control
;
_journal_issue                   14
_journal_name_full               Macromolecules
_journal_page_first              5304
_journal_paper_doi               10.1021/acs.macromol.8b00924
_journal_volume                  51
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_sum            'C51 H57 Mg N3 O2 Si2'
_chemical_formula_weight         824.48
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.371(4)
_cell_length_b                   19.871(7)
_cell_length_c                   20.675(7)
_cell_measurement_reflns_used    2336
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      36.491
_cell_measurement_theta_min      4.442
_cell_volume                     4672(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1041
_diffrn_reflns_av_unetI/netI     0.1035
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32852
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         1.421
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
; 
 Flack x determined using 1466 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.00(11)
_refine_ls_extinction_coef       0.0023(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         8688
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1367
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1251
_reflns_Friedel_coverage         0.799
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4547
_reflns_number_total             8688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma8b00924_si_002.cif
_cod_data_source_block           mo_dm15804_0m
_cod_original_cell_volume        4671(3)
_cod_database_code               1552828
_shelx_estimated_absorpt_t_min   0.972
_shelx_estimated_absorpt_t_max   0.983
_shelxl_version_number           2013-4
_shelx_res_checksum              63878
_shelx_hkl_checksum              22604
_olex2_submission_special_instructions 'No special instructions were received'