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_1552830
_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 rmad
_chemical_formula_moiety         'C50 H57 Mg N3 O2 Si2, C3.5 H4'
_chemical_formula_sum            'C53.5 H61 Mg N3 O2 Si2'
_chemical_formula_weight         858.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.551(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.162(3)
_cell_length_b                   11.2330(13)
_cell_length_c                   19.873(3)
_cell_measurement_reflns_used    2783
_cell_measurement_temperature    130
_cell_measurement_theta_max      22.89
_cell_measurement_theta_min      2.22
_cell_volume                     4892.3(11)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0764
_diffrn_reflns_av_unetI/netI     0.1230
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24531
_diffrn_reflns_point_group_measured_fraction_full 0.830
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.386
_diffrn_reflns_theta_min         1.858
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0540 before and 0.0424 after correction.
The Ratio of minimum to maximum transmission is 0.8863.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_description       block
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 1626 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.10(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         11794
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.1342
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0345P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.1039
_reflns_Friedel_coverage         0.540
_reflns_Friedel_fraction_full    0.641
_reflns_Friedel_fraction_max     0.588
_reflns_number_gt                6590
_reflns_number_total             11794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma8b00924_si_002.cif
_cod_data_source_block           dm16274
_cod_original_cell_volume        4892.2(12)
_cod_original_formula_sum        'C53.50 H61 Mg N3 O2 Si2'
_cod_database_code               1552830
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.981
_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. Others
 Fixed Sof: H51A(0.5) H51B(0.5) H51C(0.5)
3.a Ternary CH refined with riding coordinates:
 C18(H18)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C17(H17A,H17B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C20(H20),
 C21(H21), C22(H22), C23(H23), C24(H24), C28(H28), C29(H29), C30(H30), C31(H31),
  C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40),
 C41(H41), C42(H42), C43(H43), C44(H44), C53(H53), C54(H54), C55(H55)
3.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,
 H51B,H51C)
;
_shelx_res_checksum              82809
_shelx_hkl_checksum              66402
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'