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_7714670
_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 H47 Al N2 O, 2(C6 H6)'
_chemical_formula_sum            'C44 H59 Al N2 O'
_chemical_formula_weight         658.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                 98.944(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6770(2)
_cell_length_b                   12.1215(2)
_cell_length_c                   13.1408(2)
_cell_measurement_reflns_used    15968
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      68.2500
_cell_measurement_theta_min      3.3730
_cell_volume                     1994.72(6)
_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      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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   -110.00 -19.00   0.50    0.55    --  -41.33 -62.00-111.00  182
  2  \w    -64.00  27.00   0.50    0.55    --  -41.33  62.00  26.00  182
  3  \w    -26.00  64.00   0.50    0.55    --   41.33 -62.00-111.00  180
  4  \w     19.00 110.00   0.50    0.55    --   41.33  62.00  26.00  182
  5  \w    -73.00 -14.00   0.50    2.18    --  -82.50  62.00  26.00  118
  6  \w     74.00 164.00   0.50    2.18    --   96.67  62.00  26.00  180
  7  \w     28.00  73.00   0.50    2.18    --   96.67 -62.00-111.00   90
  8  \w    -28.00  30.00   0.50    0.55    --  -41.33  21.00-150.00  116
  9  \w    -48.00  26.00   0.50    0.55    --  -41.33  43.00 120.00  148
 10  \w    -34.00  24.00   0.50    0.55    --   41.33 -11.00  90.00  116
 11  \w     41.00 100.00   0.50    0.55    --   41.33-138.00-180.00  118
 12  \w    -30.00  28.00   0.50    0.55    --   41.33 -21.00  60.00  116
 13  \w    -34.00  24.00   0.50    0.55    --   41.33 -11.00-150.00  116
 14  \w    -30.00  28.00   0.50    0.55    --   41.33 -21.00-180.00  116
 15  \w   -157.00 -83.00   0.50    2.18    --  -82.50 -96.00 -30.00  148
 16  \w   -151.00 -60.00   0.50    2.18    --  -82.50 -62.00-111.00  182
 17  \w     30.00  57.00   0.50    2.18    --   96.67 -50.00 -90.00   54
 18  \w     30.00 109.00   0.50    2.18    --   96.67-117.00 150.00  158
 19  \w    105.00 170.00   0.50    2.18    --   96.67  96.00 -60.00  130
 20  \w    105.00 170.00   0.50    2.18    --   96.67  96.00 -90.00  130
 21  \w     81.00 164.00   0.50    2.18    --   96.67 145.00 120.00  166
 22  \w     30.00  57.00   0.50    2.18    --   96.67 -50.00 -60.00   54
 23  \w     29.00  68.00   0.50    2.18    --   96.67 -59.00-180.00   78
 24  \w     82.00 167.00   0.50    2.18    --   96.67  25.00   0.00  170
 25  \w     83.00 164.00   0.50    2.18    --   96.67  33.00 -60.00  162
 26  \w     81.00 164.00   0.50    2.18    --   96.67 145.00-180.00  166
 27  \w     30.00  57.00   0.50    2.18    --   96.67 -50.00   0.00   54
 28  \w     28.00 105.00   0.50    2.18    --   96.67 -77.00 120.00  154
 29  \w     29.00  68.00   0.50    2.18    --   96.67 -59.00  60.00   78
 30  \w     30.00  57.00   0.50    2.18    --   96.67 -50.00-150.00   54
 31  \w     28.00 105.00   0.50    2.18    --   96.67 -77.00-120.00  154
 32  \w     29.00  83.00   0.50    2.18    --   96.67 -68.00 -60.00  108
 33  \w     82.00 167.00   0.50    2.18    --   96.67  25.00  90.00  170
 34  \w     30.00  57.00   0.50    2.18    --   96.67 -50.00 150.00   54
 35  \w   -110.00 -14.00   0.50    0.55    --  -41.33 -77.00   0.00  192
 36  \w   -110.00 -14.00   0.50    0.55    --  -41.33 -77.00-150.00  192
 37  \w   -110.00 -14.00   0.50    0.55    --  -41.33 -77.00 -30.00  192
 38  \w   -109.00 -18.00   0.50    0.55    --  -41.33 -65.00 150.00  182
 39  \w   -110.00 -14.00   0.50    0.55    --  -41.33 -77.00  60.00  192
 40  \w    -24.00  35.00   0.50    0.55    --  -41.33  11.00  30.00  118
 41  \w   -110.00 -14.00   0.50    0.55    --  -41.33 -77.00 120.00  192
 42  \w   -110.00 -14.00   0.50    0.55    --  -41.33 -77.00 -60.00  192
 43  \w     15.00 110.00   0.50    0.55    --   41.33  77.00  90.00  190
 44  \w     25.00 109.00   0.50    0.55    --   41.33  43.00-180.00  168
 45  \w     83.00 129.00   0.50    2.18    --   96.67  33.00 150.00   92
;
_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      -0.0964504000
_diffrn_orient_matrix_UB_12      0.0674667000
_diffrn_orient_matrix_UB_13      -0.0523442000
_diffrn_orient_matrix_UB_21      0.0036601000
_diffrn_orient_matrix_UB_22      -0.0619732000
_diffrn_orient_matrix_UB_23      -0.1017526000
_diffrn_orient_matrix_UB_31      -0.0762617000
_diffrn_orient_matrix_UB_32      -0.0880314000
_diffrn_orient_matrix_UB_33      0.0316279000
_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  0.0691
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21499
_diffrn_reflns_point_group_measured_fraction_full 0.871
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.197
_diffrn_reflns_theta_min         3.405
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55736
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_description       needle
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.184
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 2166 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         6326
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0664P)^2^+0.1653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1202
_reflns_Friedel_coverage         0.655
_reflns_Friedel_fraction_full    0.730
_reflns_Friedel_fraction_max     0.723
_reflns_number_gt                5880
_reflns_number_total             6326
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02932h2.cif
_cod_data_source_block           sg_318_auto_santu01
_cod_depositor_comments
'Adding full bibliography for 7714669--7714670.cif.'
_cod_database_code               7714670
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Al'
_chemical_oxdiff_usercomment     100K
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.683
_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 Ternary CH refined with riding coordinates:
 C13(H13), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C20(H20), C22(H22), C8(H8), C00Q(H00Q), C00S(H00S),
 C00T(H00T), C00U(H00U), C7(H7), C00Y(H00Y), C00Z(H00Z), C011(H011), C6(H6),
 C016(H016), C019(H019), C01A(H01A), C01B(H01B), C01C(H01C)
2.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C28(H28A,H28B,H28C), C11(H11A,H11B,H11C), C25(H25A,
 H25B,H25C), C24(H24A,H24B,H24C), C12(H12A,H12B,H12C), C26(H26A,H26B,H26C),
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              66040
_shelx_hkl_checksum              40285
_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 1.652
_oxdiff_exptl_absorpt_empirical_full_min 0.600