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_1573382
_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         'C19 H23 Al Br2 N2 O2, C4 H8 O'
_chemical_formula_sum            'C23 H31 Al Br2 N2 O3'
_chemical_formula_weight         570.30
_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     dual
_audit_creation_date             2020-05-16
_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                 104.702(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3914(4)
_cell_length_b                   10.0911(2)
_cell_length_c                   14.2716(3)
_cell_measurement_reflns_used    16139
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      26.7870
_cell_measurement_theta_min      2.3400
_cell_volume                     2422.64(9)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_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 0.962
_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     25.00  51.00   0.50   43.27    --   10.60  77.00 -60.00   52
  2  \w     30.00  56.00   0.50   43.27    --   10.60  82.00-120.00   52
  3  \w    -13.00  16.00   0.50   43.27    --   10.60  82.00  30.00   58
  4  \w     64.00  89.00   0.50   43.27    --   10.60  77.00 -60.00   50
  5  \w     49.00  93.00   0.50   43.27    --   10.60  82.00  60.00   88
  6  \w    -76.00  47.00   0.50   43.27    --   10.60 -38.00 -30.00  246
  7  \w    -20.00  50.00   0.50   43.27    --   10.60  57.00 150.00  140
  8  \w     -7.00  99.00   0.50   43.27    --   10.60  82.00 -90.00  212
  9  \w     -3.00  23.00   0.50   43.27    --   10.60  82.00  60.00   52
 10  \w     -4.00 100.00   0.50   43.27    --   10.60  57.00-150.00  208
 11  \w    -67.00  -7.00   0.50   43.27    --   10.60 -57.00 -90.00  120
 12  \w     12.00  37.00   0.50   43.27    --   10.60 -57.00 -90.00   50
 13  \w     62.00  88.00   0.50   43.27    --   10.60  82.00-180.00   52
 14  \w    -10.00  16.00   0.50   43.27    --   10.60  82.00-180.00   52
 15  \w     73.00  98.00   0.50   43.27    --   10.60  57.00 150.00   50
 16  \w    -14.00  14.00   0.50   43.27    --   10.60  82.00-120.00   56
 17  \w    -25.00   3.00   0.50   43.27    --  -10.90 -82.00   0.00   56
 18  \w    -80.00 -55.00   0.50   43.27    --  -10.90 -82.00   0.00   50
 19  \w    -91.00 -66.00   0.50   43.27    --  -10.90 -82.00  30.00   50
 20  \w    -58.00 -33.00   0.50   43.27    --  -10.90 -82.00-120.00   50
 21  \w    -35.00  -6.00   0.50   43.27    --  -10.90  82.00 -30.00   58
 22  \w    -77.00 -13.00   0.50   43.27    --  -10.90 -77.00-180.00  128
 23  \w    -14.00  15.00   0.50   43.27    --  -10.90 -82.00  30.00   58
 24  \w    -23.00   8.00   0.50   43.27    --  -10.90 -82.00-120.00   62
;
_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      0.0347266000
_diffrn_orient_matrix_UB_12      -0.0273270000
_diffrn_orient_matrix_UB_13      0.0312973000
_diffrn_orient_matrix_UB_21      -0.0239190000
_diffrn_orient_matrix_UB_22      -0.0405333000
_diffrn_orient_matrix_UB_23      0.0218219000
_diffrn_orient_matrix_UB_31      0.0004242000
_diffrn_orient_matrix_UB_32      -0.0504853000
_diffrn_orient_matrix_UB_33      -0.0344282000
_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  0.0782
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            40413
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.081
_diffrn_reflns_theta_min         2.354
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.409
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54520
_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    1.564
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0517P)^2^+1.0933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0960
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4125
_reflns_number_total             5128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02923b3.cif
_cod_data_source_block           k10905-hyc-c
_cod_depositor_comments
'Adding full bibliography for 1573381--1573385.cif.'
_cod_database_code               1573382
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C19 H23 Br2 N2 O2 Al'
_diffrn_oxdiff_digest_frames
;
01e0a156f8e7632734035bb45ecd5c6ac0000255ffd
;
_diffrn_oxdiff_digest_hkl
;
0130a6c82f6c215cb0d98d691a591ceefaa737
;
_reflns_odcompleteness_completeness 99.94
_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:
 C1(H1a,H1b), C3(H3a,H3b), C10(H10a,H10b), C12(H12a,H12b), C20(H20b,H20a),
 C21(H21a,H21b), C22(H22a,H22b), C23(H23b,H23a)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C8(H8), C14(H14), C16(H16), C17(H17)
2.c Idealised Me refined as rotating group:
 C2(H2c,H2a,H2b), C11(H11a,H11b,H11c), C19(H19b,H19a,H19c)
;
_shelx_res_checksum              44879
_shelx_hkl_checksum              48450
_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 1.701
_oxdiff_exptl_absorpt_empirical_full_min 0.646