Random copolymerization of trimethylene carbonate with L-lactide initiated by amine-bridged bis(phenolate) neodymium alkoxides.
Hu, Guojun; Wang, Yanwei; Wang, Yaorong; Zhu, Xuehua; Yuan, Dan; Yao, Yingming; Chemical communications (Cambridge, England) 59 (2023) 6921–6924; doi:10.1039/d3cc01766d

data_7131625
_publ_section_title
;
 Random copolymerization of trimethylene carbonate with L-lactide
 initiated by amine-bridged bis(phenolate) neodymium alkoxides.
;
_journal_issue                   45
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6921
_journal_page_last               6924
_journal_paper_doi               10.1039/d3cc01766d
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         '1(C38 H60 F3 N2 Nd O7), C4 H8 O'
_chemical_formula_sum            'C42 H68 F3 N2 Nd O8'
_chemical_formula_weight         930.22
_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             2023-05-02
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2023-05-03 deposited with the CCDC.	2023-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                99.326(3)
_cell_angle_beta                 92.638(3)
_cell_angle_gamma                90.353(3)
_cell_formula_units_Z            4
_cell_length_a                   11.4516(6)
_cell_length_b                   17.9776(10)
_cell_length_c                   21.6593(12)
_cell_measurement_reflns_used    9014
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      105.190
_cell_measurement_theta_min      6.058
_cell_volume                     4395.0(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'SMART (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120.0
_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           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.1163
_diffrn_reflns_av_unetI/netI     0.0900
_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       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            101115
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        52.978
_diffrn_reflns_theta_max         52.978
_diffrn_reflns_theta_min         2.583
_diffrn_source_current           3.57
_diffrn_source_power             0.2494002
_diffrn_source_voltage           69.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.423
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.5567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1524 before and 0.0894 after correction.
The Ratio of minimum to maximum transmission is 0.7404.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             1940
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.434
_refine_diff_density_min         -2.231
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1312
_refine_ls_number_reflns         15529
_refine_ls_number_restraints     1063
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0639
_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^)+(0.0967P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1587
_refine_ls_wR_factor_ref         0.1774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10474
_reflns_number_total             15529
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01766d2.cif
_cod_data_source_block           ga220115c_0m_a
_cod_depositor_comments
'Adding full bibliography for 7131624--7131625.cif.'
_cod_database_code               7131625
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.566
_shelx_estimated_absorpt_t_min   0.360
_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
 C81-C4 \\sim C41-C4
 with sigma of 0.02
 O0AA-C45 \\sim O0AA-C9
 with sigma of 0.02
 N2-C83 \\sim N3-C31
 with sigma of 0.02
 N3-C81 \\sim N2-C41
 with sigma of 0.02
 N2-C21 \\sim N3-C17
 with sigma of 0.02
 Nd1-N3 \\sim Nd1-N2
 with sigma of 0.02
 O5-C37 \\sim O13-C11
 with sigma of 0.02
 Nd1-O5 \\sim Nd1-O13
 with sigma of 0.02
 O5-C19 \\sim O13-C85
 with sigma of 0.04
 C73-C37 \\sim C43-C11
 with sigma of 0.04
 O5-C73 \\sim O13-C43
 with sigma of 0.02
 C37-C75 \\sim C11-C87
 with sigma of 0.04
 C73-C19 \\sim C43-C85
 with sigma of 0.04
 C37-C19 \\sim C11-C85
 with sigma of 0.02
 C75-C19 \\sim C87-C85
 with sigma of 0.02
 Nd1-C73 \\sim Nd1-C43
 with sigma of 0.04
 C73-C75 \\sim C43-C87
 with sigma of 0.02
 Nd1-C37 \\sim Nd1-C11
 with sigma of 0.04
 O5-C75 \\sim O13-C87
 with sigma of 0.04
 C45-C89 \\sim C9-C71
 with sigma of 0.02
 F0AA-F14 \\sim F14-F15 \\sim F0AA-F15
 with sigma of 0.02
 O1AA-C5 \\sim O5AA-C91
 with sigma of 0.02
 C79-C65 \\sim C23-C93
 with sigma of 0.02
 Nd0A-O5AA \\sim Nd0A-O1AA
 with sigma of 0.02
 C47-C93 \\sim C77-C65
 with sigma of 0.02
 C91-C47 \\sim C5-C77
 with sigma of 0.02
 O5AA-C23 \\sim O1AA-C79
 with sigma of 0.02
 F15-C89 \\sim F0AA-C89 \\sim F14-C89
 with sigma of 0.02
 F0AA-F15 \\sim F0AA-F14 \\sim F14-F15
 with sigma of 0.02
 O3-C95 \\sim O3-C97
 with sigma of 0.02
 C95-C3 \\sim C97-C49
 with sigma of 0.02
 F1AA-C49 \\sim F3-C49 \\sim F2-C3 \\sim F11-C3 \\sim F13-C49 \\sim F1-C3
 with sigma of 0.02
 F13-C97 \\sim F3-C97 \\sim F1AA-C97
 with sigma of 0.02
 O15-C2 \\sim O11-C2
 with sigma of 0.02
 C99-C67 \\sim C39-C67
 with sigma of 0.02
 F0AA-F15 \\sim F0AA-F14 \\sim F15-F14
 with sigma of 0.02
 N5-C57 \\sim N5-C25
 with sigma of 0.02
 C6-C25 \\sim C6-C57
 with sigma of 0.02
 Nd0A-N1AA \\sim Nd0A-N5
 with sigma of 0.02
 N5-C59 \\sim N1AA-C101
 with sigma of 0.02
 N5-C69 \\sim N1AA-C51
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O5 \\sim O13 \\sim C11 \\sim C19 \\sim C37 \\sim C43 \\sim C73 \\sim C75 \\sim
C85 \\sim C87: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 3.8A
F1AA \\sim F2 \\sim F3 \\sim F1 \\sim F11 \\sim F13 \\sim O3 \\sim C3 \\sim C49
\\sim C95 \\sim C97: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.01 within 3.8A
O11 \\sim O15 \\sim C39 \\sim C99: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 3.8A
Uanis(F3AA) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(F4AA)
\\sim Ueq, Uanis(F2AA) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(F14) \\sim Ueq,
Uanis(F15) \\sim Ueq, Uanis(F0AA) \\sim Ueq, Uanis(C45) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.01
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 F0AA, F14, F15, O0AA, C45, C89
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C17, C31, C81
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, C21, C41, C83
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Nd0A, O5AA, C23, C47, C91, C93
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Nd0A, O1AA, C5, C65, C77, C79
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F2, F1, F11, O3, C3, C95
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1AA, F3, F13, O3, C49, C97
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O11, C2, C39, C67, C96
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O15, C2, C67, C96, C99
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1AA, C25, C51, C101
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, C57, C59, C69
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H4BC)=Sof(H4BD)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C41)=Sof(H41A)=
 Sof(H41B)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H83C)=1-FVAR(1)
 Sof(H4AA)=Sof(H4AB)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C31)=Sof(H31A)=
 Sof(H31B)=Sof(H31C)=Sof(C81)=Sof(H81A)=Sof(H81B)=FVAR(1)
 Sof(N2)=1-FVAR(2)
 Sof(N3)=FVAR(2)
 Sof(O13)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C85)=
 Sof(H85A)=Sof(H85B)=Sof(C87)=Sof(H87A)=Sof(H87B)=1-FVAR(3)
 Sof(O5)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C73)=
 Sof(H73A)=Sof(H73B)=Sof(C75)=Sof(H75A)=Sof(H75B)=FVAR(3)
 Sof(F0AA)=Sof(F14)=Sof(F15)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C89)=1-FVAR(4)
 Sof(F3AA)=Sof(F4AA)=Sof(F2AA)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C71)=FVAR(4)
 Sof(O5AA)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C91)=
 Sof(H91A)=Sof(H91B)=Sof(C93)=Sof(H93A)=Sof(H93B)=1-FVAR(5)
 Sof(O1AA)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(C77)=
 Sof(H77A)=Sof(H77B)=Sof(C79)=Sof(H79A)=Sof(H79B)=FVAR(5)
 Sof(F1AA)=Sof(F3)=Sof(F13)=Sof(C49)=Sof(C97)=Sof(H97A)=Sof(H97B)=1-FVAR(6)
 Sof(F2)=Sof(F1)=Sof(F11)=Sof(C3)=Sof(C95)=Sof(H95A)=Sof(H95B)=FVAR(6)
 Sof(O15)=Sof(H2BC)=Sof(H2BD)=Sof(H67C)=Sof(H67D)=Sof(C99)=Sof(H99A)=Sof(H99B)=
 1-FVAR(7)
 Sof(O11)=Sof(H2AA)=Sof(H2AB)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H67A)=Sof(H67B)=
 FVAR(7)
 Sof(H6BC)=Sof(H6BD)=Sof(C25)=Sof(H25A)=Sof(H25B)=1-FVAR(8)
 Sof(H6AA)=Sof(H6AB)=Sof(C57)=Sof(H57A)=Sof(H57B)=FVAR(8)
 Sof(N1AA)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C101)=Sof(H10A)=
 Sof(H10B)=Sof(H10C)=1-FVAR(9)
 Sof(N5)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C69)=Sof(H69A)=Sof(H69B)=
 Sof(H69C)=FVAR(9)
6.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6AA,H6AB), C6(H6BC,H6BD), C9(H9A,H9B), C23(H23A,H23B),
 C25(H25A,H25B), C26(H26A,H26B), C38(H38A,H38B), C45(H45A,H45B), C47(H47A,H47B),
  C57(H57A,H57B), C61(H61A,H61B), C65(H65A,H65B), C70(H70A,H70B), C77(H77A,
 H77B), C79(H79A,H79B), C90(H90A,H90B), C91(H91A,H91B), C93(H93A,H93B),
 C98(H98A,H98B), C4(H4AA,H4AB), C4(H4BC,H4BD), C11(H11A,H11B), C18(H18A,H18B),
 C19(H19A,H19B), C24(H24A,H24B), C29(H29A,H29B), C37(H37A,H37B), C41(H41A,H41B),
  C43(H43A,H43B), C73(H73A,H73B), C75(H75A,H75B), C81(H81A,H81B), C82(H82A,
 H82B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C95(H95A,H95B),
 C97(H97A,H97B), C102(H10G,H10H), C7(H7A,H7B), C33(H33A,H33B), C35(H35A,H35B),
 C63(H63A,H63B), C2(H2AA,H2AB), C2(H2BC,H2BD), C39(H39A,H39B), C67(H67A,H67B),
 C67(H67C,H67D), C96(H96A,H96B), C99(H99A,H99B)
6.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C30(H30), C36(H36), C48(H48), C44(H44), C52(H52), C64(H64), C68(H68)
6.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C27(H27A,H27B,H27C), C42(H42A,H42B,H42C), C51(H51A,H51B,
 H51C), C53(H53A,H53B,H53C), C59(H59A,H59B,H59C), C69(H69A,H69B,H69C), C76(H76A,
 H76B,H76C), C80(H80A,H80B,H80C), C84(H84A,H84B,H84C), C94(H94A,H94B,H94C),
 C101(H10A,H10B,H10C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C21(H21A,H21B,
 H21C), C31(H31A,H31B,H31C), C50(H50A,H50B,H50C), C54(H54A,H54B,H54C), C55(H55A,
 H55B,H55C), C62(H62A,H62B,H62C), C66(H66A,H66B,H66C), C83(H83A,H83B,H83C),
 C100(H10D,H10E,H10F), C103(H10I,H10J,H10K)
;
_olex2_submission_special_instructions 'No special instructions were received'