Evolution of aluminum aminophenolate complexes in the ring-opening polymerization of ε-caprolactone: electronic and amino-chelating effects.
Ganta, Prasanna Kumar; Huang, Fei; Halima, Taoufik Ben; Kamaraj, Rajiv; Chu, Yu-Ting; Tseng, Hsi-Ching; Ding, Shangwu; Wu, Kuo-Hui; Chen, Hsuan-Ying; Dalton transactions (Cambridge, England : 2003) 54 (2025) 511–532; doi:10.1039/d4dt02923b

data_1573384
_publ_section_title
;
 Evolution of aluminum aminophenolate complexes in the ring-opening
 polymerization of &#x3b5;-caprolactone: electronic and amino-chelating
 effects.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              511
_journal_page_last               532
_journal_paper_doi               10.1039/d4dt02923b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C40 H56 Al Cl O3'
_chemical_formula_sum            'C40 H56 Al Cl O3'
_chemical_formula_weight         647.27
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-12-15
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-03-10 deposited with the CCDC.	2024-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.6759(2)
_cell_length_b                   17.5313(3)
_cell_length_c                   40.2687(8)
_cell_measurement_reflns_used    56356
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.0250
_cell_measurement_theta_min      2.0170
_cell_volume                     7536.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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      130(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -20.00  99.32   0.38   16.25    --   10.60  57.00  90.00  314
  2  \w    -15.00  99.00   0.38   16.25    --   10.60  77.00 -60.00  300
  3  \w    -79.00  47.16   0.38   16.25    --   10.60 -37.00  90.00  332
  4  \w    -17.00  99.28   0.38   16.25    --   10.60  82.00-150.00  306
  5  \w    -17.00  99.28   0.38   16.25    --   10.60  82.00   0.00  306
  6  \w    -20.00  99.32   0.38   16.25    --   10.60  57.00 -60.00  314
  7  \w    -17.00  80.28   0.38   16.25    --   10.60  82.00  90.00  256
  8  \w     -6.00  20.22   0.38   16.25    --   10.60  82.00  60.00   69
  9  \w     59.00  85.22   0.38   16.25    --   10.60  82.00  60.00   69
 10  \w    -20.00  30.16   0.38   16.25    --   10.60  57.00-150.00  132
 11  \w     38.00  99.18   0.38   16.25    --   10.60  57.00-150.00  161
 12  \w    -85.00 -58.78   0.38   16.25    --  -10.90 -82.00   0.00   69
 13  \w    -45.00  15.04   0.38   16.25    --  -10.90 -82.00  60.00  158
 14  \w    -40.00  73.24   0.38   16.25    --  -10.90  57.00 -30.00  298
 15  \w    -20.00  15.34   0.38   16.25    --  -10.90 -82.00 150.00   93
 16  \w    -91.00 -64.78   0.38   16.25    --  -10.90 -82.00  60.00   69
 17  \w    -55.00 -28.78   0.38   16.25    --  -10.90 -82.00 150.00   69
 18  \w    -35.00  -9.92   0.38   16.25    --  -10.90  82.00-150.00   66
 19  \w    -16.00  15.92   0.38   16.25    --  -10.90 -82.00   0.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro II AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0506328000
_diffrn_orient_matrix_UB_12      0.0029599000
_diffrn_orient_matrix_UB_13      -0.0113549000
_diffrn_orient_matrix_UB_21      -0.0337631000
_diffrn_orient_matrix_UB_22      0.0221481000
_diffrn_orient_matrix_UB_23      0.0117050000
_diffrn_orient_matrix_UB_31      0.0266284000
_diffrn_orient_matrix_UB_32      0.0337151000
_diffrn_orient_matrix_UB_33      -0.0066756000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1070
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            146199
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.023
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
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    1.141
_exptl_crystal_description       block
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         6626
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0679P)^2^+8.8273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1584
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5773
_reflns_number_total             6626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02923b3.cif
_cod_data_source_block           k11112-hyc-c_auto
_cod_depositor_comments
'Adding full bibliography for 1573381--1573385.cif.'
_cod_database_code               1573384
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.925
_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(C22) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C28) \\sim Ueq,
Uanis(C32) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C14) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C15(H15)
3.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C24(H24), C5(H5), C26(H26), C21(H21), C20(H20), C17(H17), C18(H18)
3.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C13(H13A,H13B,H13C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C36(H36A,H36B,
 H36C), C34(H34A,H34B,H34C), C33(H33A,H33B,H33C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              64934
_shelx_hkl_checksum              30259
_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 2.620
_oxdiff_exptl_absorpt_empirical_full_min 0.710