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_1573383
_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         'C18 H30 Al N O2'
_chemical_formula_sum            'C18 H30 Al N O2'
_chemical_formula_weight         319.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-05-17
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_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            4
_cell_length_a                   19.0286(2)
_cell_length_b                   8.45730(10)
_cell_length_c                   11.54500(10)
_cell_measurement_reflns_used    48051
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      26.9930
_cell_measurement_theta_min      2.1400
_cell_volume                     1857.94(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_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    -16.00 100.00   0.50   14.81    --   10.60  61.00 140.00  232
  2  \w    -79.00  37.00   0.50   14.81    --   10.60 -61.00   2.00  232
  3  \w   -100.00  15.00   0.50   14.81    --  -10.90 -61.00   2.00  230
  4  \w    -37.00  78.00   0.50   14.81    --  -10.90  61.00 140.00  230
  5  \w    -17.00 100.00   0.50   14.81    --   10.60  82.00 -60.00  234
  6  \w    -79.00  36.00   0.50   14.81    --   10.60 -77.00-120.00  230
  7  \w    -17.00 100.00   0.50   14.81    --   10.60  82.00-180.00  234
  8  \w    -17.00 100.00   0.50   14.81    --   10.60  82.00-120.00  234
  9  \w    -17.00 100.00   0.50   14.81    --   10.60  82.00 -30.00  234
 10  \w   -100.00  17.00   0.50   14.81    --  -10.90 -82.00 -30.00  234
 11  \w   -100.00  17.00   0.50   14.81    --  -10.90 -82.00   0.00  234
 12  \w    -36.00  79.00   0.50   14.81    --  -10.90  77.00-150.00  230
 13  \w    -48.00  79.00   0.50   14.81    --  -10.90  38.00-120.00  254
 14  \w    -36.00  79.00   0.50   14.81    --  -10.90  77.00 150.00  230
 15  \w   -100.00  17.00   0.50   14.81    --  -10.90 -82.00 -60.00  234
 16  \w    -79.00  37.00   0.50   14.81    --   10.60 -79.00 -41.20  232
 17  \w    -79.00  38.00   0.50   14.81    --   10.60 -82.00 -60.00  234
 18  \w    -79.00  38.00   0.50   14.81    --   10.60 -82.00  90.00  234
 19  \w    -79.00  26.00   0.50   14.81    --   10.60 -78.00  44.44  210
 20  \w    -38.00  79.00   0.50   14.81    --  -10.90  82.00   0.00  234
;
_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      -0.0087386000
_diffrn_orient_matrix_UB_12      -0.0377772000
_diffrn_orient_matrix_UB_13      -0.0529226000
_diffrn_orient_matrix_UB_21      -0.0252972000
_diffrn_orient_matrix_UB_22      0.0595810000
_diffrn_orient_matrix_UB_23      -0.0114790000
_diffrn_orient_matrix_UB_31      0.0259474000
_diffrn_orient_matrix_UB_32      0.0453442000
_diffrn_orient_matrix_UB_33      -0.0290204000
_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  0.0374
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            71184
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.055
_diffrn_reflns_theta_min         2.141
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.56a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.175
_refine_diff_density_min         -0.159
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details
;
 Flack x determined using 1719 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3991
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0370P)^2^+0.2888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0665
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                3817
_reflns_number_total             3991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02923b3.cif
_cod_data_source_block           k10905-hyc-d
_cod_depositor_comments
'Adding full bibliography for 1573381--1573385.cif.'
_cod_database_code               1573383
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C18 H30 N1 O2 Al1'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              790
_shelx_hkl_checksum              65586
_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 1.449
_oxdiff_exptl_absorpt_empirical_full_min 0.657