Flexible NHC-aryloxido aluminum complex and its zwitterionic imidazolium aluminate precursor in ring-opening polymerization of ε-caprolactone.
Goswami, Santu; Mandal, Pranay; Sarkar, Subham; Mukherjee, Mainak; Pal, Samanwita; Mallick, Dibyendu; Mukherjee, Debabrata; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1346–1354; doi:10.1039/d3dt02932h

data_7714669
_publ_section_title
;
 Flexible NHC-aryloxido aluminum complex and its zwitterionic imidazolium
 aluminate precursor in ring-opening polymerization of
 &#x3b5;-caprolactone.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1346
_journal_page_last               1354
_journal_paper_doi               10.1039/d3dt02932h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C32 H43 Al Br N2 O'
_chemical_formula_sum            'C32 H43 Al Br N2 O'
_chemical_formula_weight         578.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-29
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-05-26 deposited with the CCDC.	2023-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.9690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.48000(10)
_cell_length_b                   14.13040(10)
_cell_length_c                   16.53520(10)
_cell_measurement_reflns_used    47112
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      68.2140
_cell_measurement_theta_min      2.7080
_cell_volume                     3321.43(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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     99.00 164.00   0.50    0.20    --   96.67 117.00  30.00  130
  2  \w    105.00 170.00   0.50    0.20    --   96.67  96.00 -60.00  130
  3  \w    -30.00  31.00   0.50    0.20    --   40.33 -25.00 120.00  122
  4  \w    -35.00  24.00   0.50    0.20    --   40.33 -12.00  60.00  118
  5  \w    -28.00  67.00   0.50    0.20    --   40.33 -75.00 -64.00  190
  6  \w    -26.00  57.00   0.50    0.20    --   40.33 -50.00-180.00  166
  7  \w     27.00 127.00   0.50    0.20    --   96.67 -87.00 -60.00  200
  8  \w     18.00  79.00   0.50    0.20    --   40.33-104.00 -90.00  122
  9  \w     41.00  99.00   0.50    0.20    --   40.33-138.00-150.00  116
 10  \w     44.00 127.00   0.50    0.20    --   96.67-145.00-180.00  166
 11  \w     22.00 106.00   0.50    0.20    --   96.67 -96.00-150.00  168
 12  \w     44.00 127.00   0.50    0.20    --   96.67-145.00 -90.00  166
 13  \w     44.00 127.00   0.50    0.20    --   96.67-145.00 150.00  166
 14  \w     28.00 105.00   0.50    0.20    --   96.67 -77.00 150.00  154
 15  \w     29.00  68.00   0.50    0.20    --   96.67 -59.00  90.00   78
 16  \w     29.00  83.00   0.50    0.20    --   96.67 -68.00   0.00  108
 17  \w     27.00  98.00   0.50    0.20    --   96.67 -75.00 -64.00  142
 18  \w     30.00  57.00   0.50    0.20    --   96.67 -50.00 -60.00   54
 19  \w     30.00  57.00   0.50    0.20    --   96.67 -50.00 -30.00   54
 20  \w     30.00  57.00   0.50    0.20    --   96.67 -50.00   0.00   54
 21  \w     30.00  57.00   0.50    0.20    --   96.67 -50.00  30.00   54
 22  \w     30.00  57.00   0.50    0.20    --   96.67 -50.00  60.00   54
 23  \w     29.00  83.00   0.50    0.20    --   96.67 -68.00-150.00  108
 24  \w     29.00  68.00   0.50    0.20    --   96.67 -59.00-150.00   78
 25  \w     30.00  57.00   0.50    0.20    --   96.67 -50.00-180.00   54
 26  \w     37.00 174.00   0.50    0.20    --   96.67   8.00-120.00  274
 27  \w     73.00 165.00   0.50    0.20    --   96.67  68.00-180.00  184
 28  \w     70.00 165.00   0.50    0.20    --   96.67  77.00   0.00  190
 29  \w     75.00 164.00   0.50    0.20    --   96.67  59.00-120.00  178
 30  \w     70.00 165.00   0.50    0.20    --   96.67  77.00  30.00  190
 31  \w     70.00 165.00   0.50    0.20    --   96.67  75.00  63.00  190
 32  \w     73.00 165.00   0.50    0.20    --   96.67  68.00  90.00  184
 33  \w     75.00 164.00   0.50    0.20    --   96.67  59.00 150.00  178
 34  \w     78.00 163.00   0.50    0.20    --   96.67  50.00 120.00  170
 35  \w     83.00 164.00   0.50    0.20    --   96.67  33.00   0.00  162
 36  \w     83.00 164.00   0.50    0.20    --   96.67  33.00 -60.00  162
 37  \w     14.00 109.00   0.50    0.20    --   40.33  77.00-150.00  190
 38  \w     14.00 109.00   0.50    0.20    --   40.33  77.00 -90.00  190
 39  \w     14.00 109.00   0.50    0.20    --   40.33  77.00   0.00  190
 40  \w     14.00 109.00   0.50    0.20    --   40.33  75.00  63.00  190
 41  \w     14.00 109.00   0.50    0.20    --   40.33  77.00 120.00  190
 42  \w    -67.00  29.00   0.50    0.20    --  -40.33  75.00  63.00  192
 43  \w    -43.00  26.00   0.50    0.20    --  -40.33  38.00-150.00  138
 44  \w    -31.00  30.00   0.50    0.20    --  -40.33  25.00 -90.00  122
 45  \w    -24.00  35.00   0.50    0.20    --  -40.33  12.00  30.00  118
 46  \w    -47.00 -15.00   0.50    0.20    --  -82.50  42.00  90.00   64
 47  \w    -47.00 -15.00   0.50    0.20    --  -82.50  42.00  60.00   64
 48  \w    -98.00 -13.00   0.50    0.20    --  -82.50  75.00  63.00  170
 49  \w   -105.00 -14.00   0.50    0.20    --  -82.50  77.00-120.00  182
 50  \w   -106.00 -25.00   0.50    0.20    --  -40.33 -38.00-180.00  162
 51  \w   -109.00 -13.00   0.50    0.20    --  -40.33 -77.00-120.00  192
 52  \w   -109.00 -14.00   0.50    0.20    --  -40.33 -75.00 -64.00  190
 53  \w   -107.00 -21.00   0.50    0.20    --  -40.33 -50.00 -30.00  172
 54  \w   -109.00 -13.00   0.50    0.20    --  -40.33 -77.00 150.00  192
 55  \w   -108.00 -17.00   0.50    0.20    --  -40.33 -64.00  90.00  182
 56  \w   -151.00 -55.00   0.50    0.20    --  -82.50 -77.00  30.00  192
 57  \w   -151.00 -55.00   0.50    0.20    --  -82.50 -77.00 -60.00  192
 58  \w   -151.00 -55.00   0.50    0.20    --  -82.50 -77.00 -90.00  192
 59  \w   -151.00 -55.00   0.50    0.20    --  -82.50 -77.00-120.00  192
 60  \w   -151.00 -55.00   0.50    0.20    --  -82.50 -77.00   0.00  192
 61  \w   -151.00 -55.00   0.50    0.20    --  -82.50 -77.00 120.00  192
 62  \w   -151.00 -55.00   0.50    0.20    --  -82.50 -77.00 150.00  192
 63  \w   -151.00 -55.00   0.50    0.20    --  -82.50 -77.00 -30.00  192
 64  \w   -151.00 -55.00   0.50    0.20    --  -82.50 -77.00-150.00  192
 65  \w   -151.00 -55.00   0.50    0.20    --  -82.50 -77.00-180.00  192
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0559383000
_diffrn_orient_matrix_UB_12      0.0899799000
_diffrn_orient_matrix_UB_13      0.0306603000
_diffrn_orient_matrix_UB_21      -0.0429039000
_diffrn_orient_matrix_UB_22      -0.0008022000
_diffrn_orient_matrix_UB_23      0.0783934000
_diffrn_orient_matrix_UB_31      0.0823206000
_diffrn_orient_matrix_UB_32      -0.0615535000
_diffrn_orient_matrix_UB_33      0.0438252000
_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  0.0780
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            61920
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.284
_diffrn_reflns_theta_min         3.723
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.117
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       block
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.71
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         6059
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+4.1129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5916
_reflns_number_total             6059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02932h2.cif
_cod_data_source_block           sg_252_23feb
_cod_depositor_comments
'Adding full bibliography for 7714669--7714670.cif.'
_cod_database_code               7714669
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Br Al'
_chemical_oxdiff_usercomment     '100 K'
_shelx_estimated_absorpt_t_max   0.642
_shelx_estimated_absorpt_t_min   0.315
_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(C33) = Uanis(C17) = Uanis(C34) = Uanis(C18) = Uanis(C15)
3. Others
 Fixed Sof: C17(0.5) H17(0.5) C18(0.5) H18(0.5) C33(0.5) C34(0.5)
4.a Ternary CH refined with riding coordinates:
 C28(H28), C25(H25)
4.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C10(H10), C3(H3), C8(H8), C23(H23), C21(H21), C22(H22),
 C17(H17), C18(H18)
4.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C12(H12A,H12B,H12C), C30(H30A,
 H30B,H30C), C29(H29A,H29B,H29C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              66747
_shelx_hkl_checksum              28368
_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 1.579
_oxdiff_exptl_absorpt_empirical_full_min 0.636