Highly Isoselective and Active Zinc Catalysts for rac-Lactide Polymerization: Effect of Pendant Groups of Aminophenolate Ligands
Kan, Chao; Hu, Jianwen; Huang, Yang; Wang, Haobing; Ma, Haiyan; Macromolecules 50 (2017) 7911–; doi:10.1021/acs.macromol.7b01420

data_1547592
_publ_section_title
;
 Highly Isoselective and Active Zinc Catalysts for rac-Lactide
 Polymerization: Effect of Pendant Groups of Aminophenolate Ligands
;
_journal_issue                   20
_journal_name_full               Macromolecules
_journal_page_first              7911
_journal_paper_doi               10.1021/acs.macromol.7b01420
_journal_volume                  50
_journal_year                    2017
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C47 H59 N3 O2 Si2 Zn'
_chemical_formula_sum            'C47 H59 N3 O2 Si2 Zn'
_chemical_formula_weight         819.52
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8077(10)
_cell_length_b                   17.5384(13)
_cell_length_c                   19.3310(14)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    130
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.23
_cell_volume                     4342.3(6)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0393
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30937
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.969
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0808 before and 0.0647 after correction.
The Ratio of minimum to maximum transmission is 0.8010.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.191
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Flack x determined using 3009 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.036(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8434
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+18.0393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1840
_refine_ls_wR_factor_ref         0.1952
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                7403
_reflns_number_total             8434
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma7b01420_si_001.cif
_cod_data_source_block           mo_dm15396_0m
_cod_depositor_comments
'Adding full bibliography for 1547592--1547598.cif.'
_cod_database_code               1547592
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.836
_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. Uiso/Uaniso restraints and constraints
Uanis(C36) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C24) \\sim Ueq,
Uanis(C29) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C47) \\sim Ueq,
Uanis(C43) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq,
Uanis(C5) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.004
3.a Ternary CH refined with riding coordinates:
 C11(H11)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C25(H25),
 C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34),
  C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
3.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              8690
_shelx_hkl_checksum              73388
_olex2_submission_special_instructions 'No special instructions were received'