Cation−π Interactions Accelerate the Living Cationic Ring-Opening Polymerization of Unsaturated 2-Alkyl-2-oxazolines
Van Den Broeck, Elias; Verbraeken, Bart; Dedecker, Karen; Cnudde, Pieter; Vanduyfhuys, Louis; Verstraelen, Toon; Van Hecke, Kristof; Jerca, Valentin Victor; Catak, Saron; Hoogenboom, Richard; Van Speybroeck, Veronique; Macromolecules 53 (2020) 3832–3846; doi:10.1021/acs.macromol.0c00865

data_1557996
_publ_section_title
;
 Cation&#x2212;\p Interactions Accelerate the Living Cationic Ring-Opening
 Polymerization of Unsaturated 2-Alkyl-2-oxazolines
;
_journal_issue                   10
_journal_name_full               Macromolecules
_journal_page_first              3832
_journal_page_last               3846
_journal_paper_doi               10.1021/acs.macromol.0c00865
_journal_volume                  53
_journal_year                    2020
_chemical_formula_moiety         'C7 H9 N O'
_chemical_formula_sum            'C7 H9 N O'
_chemical_formula_weight         123.15
_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     direct
_audit_creation_date             2017-03-15
_audit_creation_method
;
Olex2 1.2
(compiled Mar  2 2017 14:02:25 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.786(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.0767(3)
_cell_length_b                   15.8073(10)
_cell_length_c                   10.3549(7)
_cell_measurement_reflns_used    3298
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      74.3500
_cell_measurement_theta_min      5.1180
_cell_volume                     657.58(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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    -83.00  19.00   1.00    1.00    --  -41.80 100.00   7.00  102
  2  \w      2.00  83.00   1.00    1.00    --   41.80-100.00 -97.00   81
  3  \w    101.00 178.00   1.00    4.00    --  109.13 100.00   7.00   77
  4  \w     29.00 112.00   1.00    4.00    --  109.13-100.00 -97.00   83
  5  \w   -114.00 -14.00   1.00    1.00    --  -41.80 -57.00  90.00  100
  6  \w    -70.00  31.00   1.00    1.00    --  -41.80  57.00-120.00  101
  7  \w     26.00 109.00   1.00    4.00    --  109.13 -94.00 -30.00   83
  8  \w     37.00 138.00   1.00    4.00    --  109.13 -61.00  90.00  101
  9  \w     94.00 178.00   1.00    4.00    --  109.13 125.00-180.00   84
 10  \w     83.00 178.00   1.00    4.00    --  109.13  45.00   0.00   95
 11  \w     77.00 178.00   1.00    4.00    --  109.13  77.00 -90.00  101
 12  \w     80.00 178.00   1.00    4.00    --  109.13  61.00  90.00   98
 13  \w   -118.00  -9.00   1.00    1.00    --  -41.80 -77.00   0.00  109
 14  \w   -116.00 -17.00   1.00    1.00    --  -41.80 -38.00 150.00   99
 15  \w      1.00  83.00   1.00    1.00    --   41.80 -99.00 120.00   82
 16  \w     14.00 115.00   1.00    1.00    --   41.80  57.00 -90.00  101
 17  \w     83.00 149.00   1.00    4.00    --  109.13  45.00-120.00   66
 18  \w     80.00 178.00   1.00    4.00    --  109.13  61.00 150.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.2655671000
_diffrn_orient_matrix_UB_12      0.0662565000
_diffrn_orient_matrix_UB_13      0.0185348000
_diffrn_orient_matrix_UB_21      -0.2765657000
_diffrn_orient_matrix_UB_22      -0.0648478000
_diffrn_orient_matrix_UB_23      -0.0470504000
_diffrn_orient_matrix_UB_31      0.0115373000
_diffrn_orient_matrix_UB_32      -0.0299170000
_diffrn_orient_matrix_UB_33      0.1422140000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6186
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.107
_diffrn_reflns_theta_min         5.159
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_description       block
_exptl_crystal_F_000             264
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0886P)^2^+0.1983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1183
_reflns_number_total             1328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma0c00865_si_002.cif
_cod_data_source_block           rh074
_cod_depositor_comments
;Adding full bibliography for 1557996.cif.

 Adding full bibliography for 1557996.cif.
;
_cod_database_code               1557996
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C7 H9 N O'
_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
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
2.b :
 C7(H7)
;
_shelx_res_checksum              36915
_shelx_hkl_checksum              15794
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.463
_oxdiff_exptl_absorpt_empirical_full_min 0.706