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_7131624
_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         'C35 H51 F6 N2 Nd O6'
_chemical_formula_sum            'C35 H51 F6 N2 Nd O6'
_chemical_formula_weight         854.01
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-05-04
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2023-05-09 deposited with the CCDC.	2023-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                83.768(3)
_cell_angle_beta                 77.981(3)
_cell_angle_gamma                65.249(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5877(3)
_cell_length_b                   10.4329(4)
_cell_length_c                   21.9228(7)
_cell_measurement_reflns_used    16867
_cell_measurement_temperature    221.90(10)
_cell_measurement_theta_max      29.5700
_cell_measurement_theta_min      2.3120
_cell_volume                     1947.22(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      221.90(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4471
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -67.00  54.00   1.00    1.50    --   12.56 -19.00 -90.00  121
  2  \w    -62.00  37.00   1.00    1.50    --   12.56 -37.00  90.00   99
  3  \w    -12.00  87.00   1.00    1.50    --   12.56  37.00 -90.00   99
  4  \w     39.00 101.00   1.00    1.50    --   12.56 178.00 120.00   62
  5  \w    -20.00  26.00   1.00    1.50    --  -13.65 -99.00 -90.00   46
  6  \w    -82.00 -34.00   1.00    1.50    --  -13.65 144.00 -19.16   48
  7  \w    -62.00  37.00   1.00    1.50    --   12.56 -37.00-180.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0008627000
_diffrn_orient_matrix_UB_12      0.0268429000
_diffrn_orient_matrix_UB_13      -0.0311539000
_diffrn_orient_matrix_UB_21      -0.0067369000
_diffrn_orient_matrix_UB_22      -0.0600559000
_diffrn_orient_matrix_UB_23      -0.0091108000
_diffrn_orient_matrix_UB_31      -0.0825440000
_diffrn_orient_matrix_UB_32      0.0357880000
_diffrn_orient_matrix_UB_33      0.0064043000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28103
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.900
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.405
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       block
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         7945
_refine_ls_number_restraints     227
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0455P)^2^+0.9269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7127
_reflns_number_total             7945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01766d2.cif
_cod_data_source_block           g230503b_autored
_cod_depositor_comments
'Adding full bibliography for 7131624--7131625.cif.'
_cod_original_cell_volume        1947.21(13)
_cod_database_code               7131624
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O6-C56A \\sim O6-C56
 with sigma of 0.02
 Nd1-O4 \\sim Nd1-O3A
 with sigma of 0.02
 O4-C7 \\sim O3A-C54A \\sim C54A-C47A \\sim C7-C47 \\sim C47A-C46A \\sim
C47-C46 \\sim C46A-C45A \\sim C46-
 C45 \\sim O4-C45 \\sim O3A-C45A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O4 \\sim C7 \\sim C45 \\sim C46 \\sim C47: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 3.8A
O3A \\sim C45A \\sim C46A \\sim C47A \\sim C54A: within 3.8A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 3.8A
4. Rigid body (RIGU) restrains
 O3A, C45A, C46A, C47A, C54A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O4, C7, C45, C46, C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(C56A)=Sof(H56D)=Sof(H56E)=Sof(H56F)=1-FVAR(1)
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=FVAR(1)
 Sof(O3A)=Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46C)=Sof(H46D)=
 Sof(C47A)=Sof(H47C)=Sof(H47D)=Sof(C54A)=Sof(H54A)=Sof(H54B)=1-FVAR(2)
 Sof(O4)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=
 Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=Sof(H47B)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C50(H50)
6.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C13(H13A,H13B), C28(H28A,H28B), C35(H35A,H35B), C43(H43A,H43B),
 C45(H45A,H45B), C45A(H45C,H45D), C46(H46A,H46B), C46A(H46C,H46D), C47(H47A,
 H47B), C47A(H47C,H47D), C54A(H54A,H54B)
6.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C19(H19), C26(H26), C29(H29)
6.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C24(H24A,H24B,H24C), C31(H31A,H31B,H31C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C49(H49A,H49B,H49C), C52(H52A,H52B,H52C), C53(H53A,
 H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C56A(H56D,H56E,H56F)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 22.984
_oxdiff_exptl_absorpt_empirical_full_min 0.763