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_1569362
_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         'C12 H30 Al N'
_chemical_formula_sum            'C12 H30 Al N'
_chemical_formula_weight         215.35
_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             2020-02-26
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-02-26 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                   7.5824(2)
_cell_length_b                   12.9289(3)
_cell_length_c                   15.4855(3)
_cell_measurement_reflns_used    3673
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.6470
_cell_measurement_theta_min      4.4480
_cell_volume                     1518.08(6)
_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  'XL  (Sheldrick, 2008)'
_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            HyPix
_diffrn_measured_fraction_theta_full 0.996
_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    -34.00  16.00   0.50    0.05    --  -47.45  34.00 -93.00  100
  2  \w    -16.00  24.00   0.50    0.05    --  -47.45  19.00-180.00   80
  3  \w    -41.00 -16.00   0.50    0.07    --  -86.25  34.00 -93.00   50
  4  \w    -66.00 -40.00   0.50    0.07    --  -86.25 133.00 -47.00   52
  5  \w    -70.00 -44.00   0.50    0.07    --  -86.25 135.00 130.00   52
  6  \w    -18.00  30.00   0.50    0.05    --   47.45 -37.00  60.00   96
  7  \w     36.00  63.00   0.50    0.07    --  107.11 -57.00 150.00   54
  8  \w     35.00  60.00   0.50    0.07    --  107.11 -57.00  90.00   50
  9  \w     37.00  62.00   0.50    0.07    --  107.11 -57.00 120.00   50
 10  \w     37.00 110.00   0.50    0.07    --  107.11-125.00  30.00  146
 11  \w     43.00 102.00   0.50    0.07    --  107.11 -77.00-120.00  118
 12  \w    107.00 162.00   0.50    0.07    --  107.11  88.00  66.00  110
 13  \w   -114.00 -76.00   0.50    0.05    --  -47.45-133.00-115.00   76
 14  \w   -153.00-121.00   0.50    0.07    --  -86.25 -37.00  30.00   64
 15  \w   -159.00-134.00   0.50    0.07    --  -86.25 -57.00-180.00   50
;
_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      -0.1811834000
_diffrn_orient_matrix_UB_12      -0.0173310000
_diffrn_orient_matrix_UB_13      -0.0427455000
_diffrn_orient_matrix_UB_21      -0.0267101000
_diffrn_orient_matrix_UB_22      0.1179022000
_diffrn_orient_matrix_UB_23      -0.0052939000
_diffrn_orient_matrix_UB_31      0.0877551000
_diffrn_orient_matrix_UB_32      0.0011377000
_diffrn_orient_matrix_UB_33      -0.0897124000
_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  0.0371
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6059
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.863
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.060
_diffrn_reflns_theta_min         4.455
_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    0.920
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
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    0.942
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_recrystallization_method 'used as received'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 958 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0700P)^2^+0.1090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1047
_reflns_Friedel_coverage         0.587
_reflns_Friedel_fraction_full    0.845
_reflns_Friedel_fraction_max     0.756
_reflns_number_gt                2643
_reflns_number_total             2769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py00482a2.cif
_cod_data_source_block           rf220e
_cod_depositor_comments
'Adding full bibliography for 1569361--1569362.cif.'
_cod_database_code               1569362
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C12NAlH30
_chemical_oxdiff_usercomment     Pr3NAlMe3
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.867
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              47950
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop with paratone oil'
_olex2_submission_original_sample_id Pr2NAlMe3
_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 1.706
_oxdiff_exptl_absorpt_empirical_full_min 0.606