Catalytic Synergy Using Al(III) and Group 1 Metals to Accelerate Epoxide and Anhydride Ring-Opening Copolymerizations
Diment, Wilfred T.; Gregory, Georgina L.; Kerr, Ryan W. F.; Phanopoulos, Andreas; Buchard, Antoine; Williams, Charlotte K.; ACS Catalysis  (2021) 12532–12542; doi:10.1021/acscatal.1c04020

data_4519053
_publ_section_title
;
 Catalytic Synergy Using Al(III) and Group 1 Metals to Accelerate Epoxide
 and Anhydride Ring-Opening Copolymerizations
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              12532
_journal_page_last               12542
_journal_paper_doi               10.1021/acscatal.1c04020
_journal_year                    2021
_chemical_formula_moiety         'C25 H30 Al Cs N2 O8, C H Cl3'
_chemical_formula_sum            'C26 H31 Al Cl3 Cs N2 O8'
_chemical_formula_weight         765.77
_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     dual
_audit_creation_date             2020-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.5770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9518(2)
_cell_length_b                   12.88710(10)
_cell_length_c                   16.7675(2)
_cell_measurement_reflns_used    10406
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      76.9830
_cell_measurement_theta_min      2.9950
_cell_volume                     3194.72(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_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 -43.00   1.00    1.00    --    0.00-178.00  30.00   56
  2  \w    -77.00 -43.00   1.00    1.00    --    0.00 178.00-150.00   34
  3  \w     -3.00  33.00   1.00    2.00    --  -60.50  15.00 120.00   36
  4  \w     -3.00  32.00   1.00    2.00    --  -60.50  15.00 -90.00   35
  5  \w   -150.00-111.00   1.00    2.00    --  -60.50 -94.00 -90.00   39
  6  \w      4.00  31.00   1.00    2.00    --  -60.50  15.00-150.00   27
  7  \w     -1.00  28.00   1.00    2.00    --  -60.50  15.00-120.00   29
  8  \w    -14.00  22.00   1.00    2.00    --  -60.50  30.00   0.00   36
  9  \w     -3.00  32.00   1.00    2.00    --  -60.50  15.00 -30.00   35
 10  \w     99.00 149.00   1.00    2.00    --   60.50 125.00-150.00   50
 11  \w     99.00 133.00   1.00    2.00    --   60.50 125.00  60.00   34
 12  \w    109.00 146.00   1.00    2.00    --   60.50 125.00   0.00   37
 13  \w    103.00 167.00   1.00    4.00    --  121.00  77.00  60.00   64
 14  \w     76.00 102.00   1.00    4.00    --  121.00 -91.00  90.00   26
 15  \w     26.00  52.00   1.00    4.00    --  121.00 -91.00  90.00   26
 16  \w    115.00 162.00   1.00    4.00    --  121.00  63.00  90.00   47
 17  \w    103.00 178.00   1.00    4.00    --  121.00  77.00 -60.00   75
 18  \w    114.00 177.00   1.00    4.00    --  121.00  77.00 -90.00   63
 19  \w     48.00  76.00   1.00    4.00    --  121.00 -50.00  60.00   28
 20  \w    105.00 177.00   1.00    4.00    --  121.00  77.00   0.00   72
 21  \w     42.00  96.00   1.00    4.00    --  121.00 -63.00-120.00   54
 22  \w     89.00 120.00   1.00    4.00    --  121.00  50.00   0.00   31
 23  \w     40.00  78.00   1.00    4.00    --  121.00 -50.00 -90.00   38
 24  \w     84.00 177.00   1.00    4.00    --  121.00  63.00  30.00   93
 25  \w     80.00 106.00   1.00    4.00    --  121.00  63.00  90.00   26
 26  \w     45.00  80.00   1.00    1.00    --    0.00  19.00 -60.00   35
 27  \w      2.00  39.00   1.00    1.00    --    0.00 -77.00  90.00   37
 28  \w    -63.00 -38.00   1.00    1.00    --    0.00 178.00-150.00   25
 29  \w      2.00  34.00   1.00    1.00    --    0.00  19.00 -60.00   32
 30  \w     -2.00  24.00   1.00    2.00    --  -60.50  30.00-120.00   26
 31  \w    -14.00   8.00   1.00    2.00    --  -60.50  30.00-150.00   22
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1006973000
_diffrn_orient_matrix_UB_12      0.0240226000
_diffrn_orient_matrix_UB_13      -0.0284345000
_diffrn_orient_matrix_UB_21      -0.0022565000
_diffrn_orient_matrix_UB_22      -0.0824486000
_diffrn_orient_matrix_UB_23      -0.0667852000
_diffrn_orient_matrix_UB_31      -0.0268623000
_diffrn_orient_matrix_UB_32      -0.0831125000
_diffrn_orient_matrix_UB_33      0.0580133000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15348
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.851
_diffrn_reflns_theta_min         2.989
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.029
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.179
_refine_diff_density_max         0.697
_refine_diff_density_min         -1.290
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         6656
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0280
_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^)+(0.0392P)^2^+1.6830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6283
_reflns_number_total             6656
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c04020_si_002.cif
_cod_data_source_block           016rwfk20
_cod_database_code               4519053
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C25H33Al1Cs1N2O8
_shelx_estimated_absorpt_t_max   0.222
_shelx_estimated_absorpt_t_min   0.146
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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. Restrained distances
 Cl2S-C1S \\sim Cl2T-C1S
 with sigma of 0.02
 Cl4S-C1S \\sim Cl4T-C1S
 with sigma of 0.02
 Cl3S-C1S \\sim Cl3T-C1S
 with sigma of 0.02
3. Others
 Sof(H1SA)=Sof(Cl2T)=Sof(Cl4T)=Sof(Cl3T)=1-FVAR(1)
 Sof(Cl2S)=Sof(Cl4S)=Sof(Cl3S)=Sof(H1S)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C1S(H1SA), C1S(H1S)
4.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C9(H9A,H9B)
4.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C8(H8), C16(H16), C18(H18), C5(H5), C3(H3), C17(H17), C4(H4)
4.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C25(H25A,H25B,H25C), C21(H21A,H21B,
 H21C), C1(H1A,H1B,H1C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              34375
_shelx_hkl_checksum              43338
_ins_header
;
TITL 016RWFK20 in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  14.951813  12.887117  16.767502  90.0000  98.5772  90.0000
ZERR    5.00   0.000167   0.000135   0.000183   0.0000   0.0010   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N O Al Cs
UNIT 125.00 165.00 10.00 40.00 5.00 5.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id 016RWFK20
_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 1.303
_oxdiff_exptl_absorpt_empirical_full_min 0.786