Highly heteroselective ring-opening polymerization of rac-lactide initiated by rare-earth alkoxides bearing chiral [NNOO]-type amine-bis(phenolate) ligands
Duan, Yu-Lai; Guo, Qian; Liu, Gui-Yang; Yi, Zhong-Zhou; Feng, Shao-Ping; Huang, Yong; Polymer Chemistry 13 (2022) 4249–4259; doi:10.1039/D2PY00455K

data_1567255
_publ_section_title
;
 Highly heteroselective ring-opening polymerization of rac-lactide
 initiated by rare-earth alkoxides bearing chiral [NNOO]-type
 amine-bis(phenolate) ligands
;
_journal_issue                   29
_journal_name_full               'Polymer Chemistry'
_journal_page_first              4249
_journal_page_last               4259
_journal_paper_doi               10.1039/D2PY00455K
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C44 H73 N2 O4 Y'
_chemical_formula_sum            'C44 H73 N2 O4 Y'
_chemical_formula_weight         782.95
_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_date             2022-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-23 deposited with the CCDC.	2022-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                94.27(3)
_cell_angle_beta                 104.50(3)
_cell_angle_gamma                90.69(3)
_cell_formula_units_Z            2
_cell_length_a                   9.938(2)
_cell_length_b                   12.053(2)
_cell_length_c                   19.598(4)
_cell_measurement_reflns_used    3686
_cell_measurement_temperature    300.79(10)
_cell_measurement_theta_max      68.9850
_cell_measurement_theta_min      4.5900
_cell_volume                     2265.3(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300.79(10)
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.1175
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15246
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.860
_diffrn_reflns_theta_min         4.516
_exptl_absorpt_coefficient_mu    2.107
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91918
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.785
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         8258
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0659
_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^)+(0.0219P)^2^+0.5189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1492
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5960
_reflns_number_total             8258
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2py00455k2.cif
_cod_data_source_block           dyl12
_cod_depositor_comments
'Adding full bibliography for 1567255--1567256.cif.'
_cod_original_cell_volume        2265.2(8)
_cod_database_code               1567255
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C16'-C15 \\sim C16-C15
 with sigma of 0.02
 C16'-C17 \\sim C17'-C16
 with sigma of 0.02
 C18-C17' \\sim C18'-C17
 with sigma of 0.02
 C18-C19 \\sim C18'-C19'
 with sigma of 0.02
 N2-C19 \\sim N2-C19'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C44' \\sim C44 \\sim C43' \\sim C43 \\sim C42' \\sim C42 \\sim C41' \\sim C41:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C30 \\sim C33 \\sim C31' \\sim C31 \\sim C32' \\sim C32 \\sim C33': within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20) \\sim Ueq, Uanis(C20') \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C39) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Same fragment restrains
{C33, C31, C32} sigma for 1-2: 0.01, 1-3: 0.02
as
{C31', C32', C33'}
{C44', C43', C42', C41'} sigma for 1-2: 0.01, 1-3: 0.02
as
{C44, C43, C42, C41}
5. Others
 Sof(H15C)=Sof(H15D)=Sof(C16')=Sof(H16')=Sof(C17')=Sof(H17A)=Sof(H17B)=
 Sof(C20')=Sof(H20A)=Sof(H20B)=Sof(C19')=Sof(H19C)=Sof(H19D)=Sof(C21')=
 Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C18')=Sof(H18C)=Sof(H18D)=1-FVAR(1)
 Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17C)=Sof(H17D)=Sof(C19)=
 Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20C)=Sof(H20D)=Sof(C21)=Sof(H21A)=Sof(H21B)=
 Sof(H21C)=Sof(C18)=Sof(H18A)=Sof(H18B)=FVAR(1)
 Sof(C44')=Sof(H44A)=Sof(H44B)=Sof(C43')=Sof(H43A)=Sof(H43B)=Sof(C42')=
 Sof(H42A)=Sof(H42B)=Sof(C41')=Sof(H41A)=Sof(H41B)=1-FVAR(2)
 Sof(C44)=Sof(H44C)=Sof(H44D)=Sof(C43)=Sof(H43C)=Sof(H43D)=Sof(C42)=Sof(H42C)=
 Sof(H42D)=Sof(C41)=Sof(H41C)=Sof(H41D)=FVAR(2)
 Sof(C31')=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C32')=Sof(H32D)=Sof(H32E)=
 Sof(H32F)=Sof(C33')=Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(3)
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C38(H38), C16(H16), C16'(H16')
6.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C44'(H44A,H44B), C43'(H43A,H43B), C42'(H42A,H42B),
 C41'(H41A,H41B), C44(H44C,H44D), C43(H43C,H43D), C42(H42C,H42D), C41(H41C,
 H41D), C15(H15A,H15B), C15(H15C,H15D), C17'(H17A,H17B), C17(H17C,H17D),
 C20'(H20A,H20B), C19(H19A,H19B), C19'(H19C,H19D), C20(H20C,H20D), C18(H18A,
 H18B), C18'(H18C,H18D)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C12(H12), C10(H10)
6.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C33(H33A,H33B,H33C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C31'(H31D,H31E,H31F), C32'(H32D,H32E,H32F),
 C33'(H33D,H33E,H33F), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C36(H36A,H36B,
 H36C), C40(H40A,H40B,H40C), C39(H39A,H39B,H39C), C21(H21A,H21B,H21C),
 C21'(H21D,H21E,H21F)
;
_shelx_res_checksum              23538
_shelx_hkl_checksum              2574
_olex2_submission_special_instructions 'No special instructions were received'