Efficient and Well-Controlled Ring Opening Polymerization of Biobased Ethylene Brassylate by α-Diimine FeCl3 Catalysts via a Coordination-Insertion Mechanism
Liu, Lijia; Zhang, Chunyu; Zhang, Xuequan; Liu, Heng; Wang, Feng; Dalton Transactions  (2023) –; doi:10.1039/D3DT02918B

data_7714451
_publ_section_title
;
 Efficient and Well-Controlled Ring Opening Polymerization of Biobased
 Ethylene Brassylate by \a-Diimine FeCl3 Catalysts via a
 Coordination-Insertion Mechanism
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02918B
_journal_year                    2023
_chemical_formula_moiety         'C54 H44 Cl3 Fe N2, 0.5[CH2Cl2]'
_chemical_formula_sum            'C54 H44 Cl3 Fe N2'
_chemical_formula_weight         883.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-12-28
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-03-06 deposited with the CCDC.	2023-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.536(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0615(2)
_cell_length_b                   18.6688(6)
_cell_length_c                   28.0754(6)
_cell_measurement_reflns_used    7813
_cell_measurement_temperature    300
_cell_measurement_theta_max      71.7420
_cell_measurement_theta_min      3.8960
_cell_volume                     4744.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      300
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.945
_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    -52.00  24.00   1.00    1.50    --  -48.20  47.00  97.00   76
  2  \w   -118.00 -35.00   1.00    1.50    --  -48.20 -47.00 -51.00   83
  3  \w     35.00  99.00   1.00    1.50    --   48.20  47.00  97.00   64
  4  \w     -9.00  16.00   1.00    1.50    --   48.20 -47.00 -51.00   25
  5  \w   -113.00 -87.00   1.00    1.50    --  -48.20-125.00-120.00   26
  6  \w    -27.00  26.00   1.00    1.50    --  -48.20  19.00-120.00   53
  7  \w   -100.00 -74.00   1.00   20.00    --  -86.25 -47.00 -51.00   26
  8  \w    -52.00 -27.00   1.00   20.00    --  -86.25  47.00  97.00   25
  9  \w    -41.00 -15.00   1.00   20.00    --  -86.25  38.00-150.00   26
 10  \w    -43.00 -13.00   1.00   20.00    --  -86.25  38.00-180.00   30
 11  \w     94.00 178.00   1.00   20.00    --  106.49  47.00  97.00   84
 12  \w     35.00  65.00   1.00   20.00    --  106.49 -57.00-150.00   30
 13  \w     36.00  66.00   1.00   20.00    --  106.49 -57.00  30.00   30
 14  \w     35.00  60.00   1.00   20.00    --  106.49 -57.00  90.00   25
 15  \w     34.00 105.00   1.00   20.00    --  106.49 -77.00 -60.00   71
 16  \w     34.00 105.00   1.00   20.00    --  106.49 -77.00 120.00   71
 17  \w     97.00 178.00   1.00   20.00    --  106.49 125.00 -30.00   81
 18  \w     36.00 105.00   1.00   20.00    --  106.49 -77.00  30.00   69
 19  \w     93.00 178.00   1.00   20.00    --  106.49  38.00-180.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0786402000
_diffrn_orient_matrix_UB_12      0.0444978000
_diffrn_orient_matrix_UB_13      -0.0397589000
_diffrn_orient_matrix_UB_21      0.1506351000
_diffrn_orient_matrix_UB_22      0.0192986000
_diffrn_orient_matrix_UB_23      -0.0199508000
_diffrn_orient_matrix_UB_31      -0.0090382000
_diffrn_orient_matrix_UB_32      -0.0667821000
_diffrn_orient_matrix_UB_33      -0.0322065000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            31028
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.521
_diffrn_reflns_theta_min         2.843
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.379
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       needle
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.382
_refine_diff_density_min         -1.757
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         9435
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0909
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2760
_refine_ls_wR_factor_ref         0.2994
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6537
_reflns_number_total             9435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02918b2.cif
_cod_data_source_block           llj_4
_cod_database_code               7714451
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.669
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl3-Cl2 \\sim Cl3A-Cl2A
 with sigma of 0.02
 Cl2-Cl1 \\sim Cl2A-Cl1A
 with sigma of 0.02
 Cl1-Cl3 \\sim Cl1A-Cl3A
 with sigma of 0.02
 Fe1-Cl3 \\sim Fe1A-Cl3A
 with sigma of 0.02
 Fe1A-Cl2A \\sim Fe1-Cl2
 with sigma of 0.02
 Fe1-Cl1 \\sim Fe1A-Cl1A
 with sigma of 0.02
 Cl2-Cl3 \\sim Cl2A-Cl3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Fe1 \\sim Cl1 \\sim Cl2 \\sim Cl3 \\sim Fe1A \\sim Cl3A \\sim Cl2A \\sim Cl1A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 Fe1, Cl2, Cl3, Cl1, N2, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Fe1A, Cl2A, Cl1A, Cl3A, N2, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(Fe1A)=Sof(Cl3A)=Sof(Cl2A)=Sof(Cl1A)=1-FVAR(1)
 Sof(Fe1)=Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C9(H9), C42(H42)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26), C28(H28),
  C29(H29), C30(H30), C36(H36), C38(H38), C44(H44), C45(H45), C46(H46),
 C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 84 electrons were 
found in a volume of 654\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.5[CH2Cl2] per Asymmetric Unit 
which account for 84 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              22030
_shelx_fab_checksum              11064
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.323
_oxdiff_exptl_absorpt_empirical_full_min 0.695