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_1573381
_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         'C21 H29 Al N2 O4'
_chemical_formula_sum            'C22 H29 Al N O4'
_chemical_formula_weight         398.44
_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     dual
_audit_creation_date             2019-10-28
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2023-01-13 deposited with the CCDC.	2024-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                79.573(5)
_cell_angle_beta                 86.427(5)
_cell_angle_gamma                88.799(5)
_cell_formula_units_Z            2
_cell_length_a                   7.0781(4)
_cell_length_b                   11.3798(6)
_cell_length_c                   12.8321(8)
_cell_measurement_reflns_used    4891
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      26.5090
_cell_measurement_theta_min      1.6550
_cell_volume                     1014.50(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.36a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.36a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.36a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(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 0.941
_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     -9.00  17.00   0.50   11.91    --   10.60  82.00 -30.00   52
  2  \w    -17.00 100.00   0.50   11.91    --   10.60  82.00 -60.00  234
  3  \w     32.00  58.00   0.50   11.91    --   10.60  57.00  60.00   52
  4  \w    -79.00 -54.00   0.50   11.91    --   10.60 -57.00 150.00   50
  5  \w     -8.00  22.00   0.50   11.91    --   10.60  57.00  60.00   60
  6  \w    -12.00 100.00   0.50   11.91    --   10.60  38.00 150.00  224
  7  \w     -3.00  43.00   0.50   11.91    --   10.60  82.00 120.00   92
  8  \w    -14.00  31.00   0.50   11.91    --   10.60  82.00-150.00   90
  9  \w     52.00  78.00   0.50   11.91    --   10.60  82.00-150.00   52
 10  \w    -13.00  30.00   0.50   11.91    --   10.60  82.00  60.00   86
 11  \w    -27.00  41.00   0.50   11.91    --   10.60 -57.00 150.00  136
 12  \w     47.00  99.00   0.50   11.91    --   10.60  77.00-120.00  104
 13  \w    -98.00 -73.00   0.50   11.91    --  -10.90 -38.00 -90.00   50
 14  \w    -92.00 -60.00   0.50   11.91    --  -10.90 -82.00-150.00   64
 15  \w    -20.00   5.00   0.50   11.91    --  -10.90 -82.00  90.00   50
 16  \w    -14.00  26.00   0.50   11.91    --  -10.90 -38.00 -90.00   80
 17  \w    -98.00 -31.00   0.50   11.91    --  -10.90 -77.00-120.00  134
;
_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      0.0312221000
_diffrn_orient_matrix_UB_12      0.0499578000
_diffrn_orient_matrix_UB_13      -0.0381889000
_diffrn_orient_matrix_UB_21      -0.0306214000
_diffrn_orient_matrix_UB_22      0.0387011000
_diffrn_orient_matrix_UB_23      0.0353760000
_diffrn_orient_matrix_UB_31      0.0903878000
_diffrn_orient_matrix_UB_32      -0.0048399000
_diffrn_orient_matrix_UB_33      0.0214530000
_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  0.0738
_diffrn_reflns_av_unetI/netI     0.0897
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13393
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.008
_diffrn_reflns_theta_min         1.616
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.36a (Rigaku Oxford Diffraction, 2019)
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    1.304
_exptl_crystal_description       block
_exptl_crystal_F_000             426
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.020(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0679
_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^)+(0.1141P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.1935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2881
_reflns_number_total             4162
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02923b3.cif
_cod_data_source_block           chen-n2o2al
_cod_depositor_comments
'Adding full bibliography for 1573381--1573385.cif.'
_cod_database_code               1573381
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C19 H23 N2 O4 Al1'
_diffrn_oxdiff_digest_frames
;
018ad0ed9619276e1c7a4b6a672648106500025715a
;
_diffrn_oxdiff_digest_hkl
;
0148df6ca2ce3dbd8de5160d50118043f60655
;
_reflns_odcompleteness_completeness 98.74
_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:
 C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C10(H10), C16(H16), C17(H17), C19(H19)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C12(H12A,H12B,H12C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C)
;
_shelx_res_checksum              641
_shelx_hkl_checksum              68575
_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 2.246
_oxdiff_exptl_absorpt_empirical_full_min 0.284