Diastereoselective synthesis of chiral aminophenolate magnesium complexes and their application in the stereoselective polymerization of rac-lactide and rac-β-butyrolactone.
Wang, Haobing; Guo, Jianshuang; Yang, Yang; Ma, Haiyan; Dalton transactions (Cambridge, England : 2003) 45 (2016) 10942–10953; doi:10.1039/c6dt01126h

data_7039368
_publ_section_title
;
 Diastereoselective synthesis of chiral aminophenolate magnesium complexes
 and their application in the stereoselective polymerization of
 rac-lactide and rac-\b-butyrolactone.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10942
_journal_page_last               10953
_journal_paper_doi               10.1039/c6dt01126h
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_sum            'C55 H73 Mg N3 O Si3'
_chemical_formula_weight         900.74
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-02-01 deposited with the CCDC.
2016-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0092(4)
_cell_length_b                   22.1908(9)
_cell_length_c                   23.6773(9)
_cell_measurement_reflns_used    1387
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      56.29
_cell_measurement_theta_min      3.73
_cell_volume                     5259.0(4)
_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      140(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1762
_diffrn_reflns_av_unetI/netI     0.1388
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            49130
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.010
_diffrn_reflns_theta_min         3.734
_exptl_absorpt_coefficient_mu    1.242
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
; 
 Flack x determined using 2221 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_coef       0.0052(5)
_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   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         9521
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0704P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1605
_reflns_Friedel_coverage         0.765
_reflns_Friedel_fraction_full    0.968
_reflns_Friedel_fraction_max     0.929
_reflns_number_gt                6402
_reflns_number_total             9521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01126h2.cif
_cod_data_source_block           cu_dm13700_0m
_cod_depositor_comments
'Adding full bibliography for 7039365--7039368.cif.'
_cod_database_code               7039368
_shelx_estimated_absorpt_t_min   0.886
_shelx_estimated_absorpt_t_max   0.988
_shelxl_version_number           2013-4
_shelx_res_checksum              85455