Unveiling the mechanisms of epoxide polymerization with N–Al adduct catalysts: a comprehensive experimental and theoretical investigation
Safaie, Niloofar; Rodriguez, Austin; Jana, Gourhari; Smak, Jessica; Mendoza-Cortes, Jose L.; Ferrier, Robert C.; Polymer Chemistry 14 (2023) 3213–3224; doi:10.1039/D3PY00482A

data_1569361
_publ_section_title
;
 Unveiling the mechanisms of epoxide polymerization with N--Al adduct
 catalysts: a comprehensive experimental and theoretical investigation
;
_journal_issue                   27
_journal_name_full               'Polymer Chemistry'
_journal_page_first              3213
_journal_page_last               3224
_journal_paper_doi               10.1039/D3PY00482A
_journal_volume                  14
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C16 H34 Al N'
_chemical_formula_sum            'C16 H34 Al N'
_chemical_formula_weight         267.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-25
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-02-25 deposited with the CCDC.	2023-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.25651(12)
_cell_length_b                   14.5203(2)
_cell_length_c                   16.1412(2)
_cell_measurement_reflns_used    4459
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.1760
_cell_measurement_theta_min      4.0620
_cell_volume                     1700.75(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.8852
_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  10.00   0.50    0.05    --   47.45  -4.00 -73.00   70
  2  \w      8.00  56.00   0.50    0.05    --   47.45 -77.00-150.00   96
  3  \w     35.00  60.00   0.50    0.05    --  107.11 -57.00-150.00   50
  4  \w     64.00 102.00   0.50    0.05    --  107.11 -77.00-180.00   76
  5  \w     78.00 106.00   0.50    0.05    --  107.11 -99.00 -60.00   56
  6  \w     38.00  64.00   0.50    0.05    --  107.11 -99.00 -60.00   52
  7  \w     35.00  60.00   0.50    0.05    --  107.11 -57.00 -90.00   50
  8  \w     35.00  60.00   0.50    0.05    --  107.11 -57.00  60.00   50
  9  \w     79.00 176.00   0.50    0.05    --  107.11   4.00 103.00  194
 10  \w     50.00  89.00   0.50    0.05    --  107.11-132.00  88.00   78
 11  \w    -20.00  22.00   0.50    0.05    --  -47.45  19.00-180.00   84
 12  \w    -28.00  20.00   0.50    0.05    --  -47.45  19.00 -90.00   96
 13  \w    -46.00 -21.00   0.50    0.05    --  -86.25   4.00 103.00   50
 14  \w   -151.00-116.00   0.50    0.05    --  -86.25-142.00   4.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0118901000
_diffrn_orient_matrix_UB_12      0.0887736000
_diffrn_orient_matrix_UB_13      -0.0519599000
_diffrn_orient_matrix_UB_21      -0.0029572000
_diffrn_orient_matrix_UB_22      0.0578025000
_diffrn_orient_matrix_UB_23      0.0800413000
_diffrn_orient_matrix_UB_31      0.2119686000
_diffrn_orient_matrix_UB_32      0.0056811000
_diffrn_orient_matrix_UB_33      -0.0017388000
_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  0.0565
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6653
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.052
_diffrn_reflns_theta_min         4.095
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           1
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.333
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.044
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_recrystallization_method 'used as recieved'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.281
_exptl_crystal_size_min          0.153
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 1110 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_coef       0.0027(8)
_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   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0570P)^2^+0.1812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.0976
_reflns_Friedel_coverage         0.599
_reflns_Friedel_fraction_full    0.864
_reflns_Friedel_fraction_max     0.783
_reflns_number_gt                3041
_reflns_number_total             3177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py00482a2.cif
_cod_data_source_block           rf220c
_cod_depositor_comments
'Adding full bibliography for 1569361--1569362.cif.'
_cod_original_cell_volume        1700.75(5)
_cod_database_code               1569361
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     MeCy2NAlMe3
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.713
_diffrn_oxdiff_digest_frames
;
0181c43145f1d47941962e723aad76b40a010721904
;
_diffrn_oxdiff_digest_hkl
;
01c88dfe722aa2582b790c874cb1964257094a
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C2(H2), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              16678
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'solvent frozen at liquid nitrogen on nylon loop '
_olex2_submission_original_sample_id MeCy2NAlMe3
_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 1.616
_oxdiff_exptl_absorpt_empirical_full_min 0.459