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_4519050
_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 N2 Na O8, 2(C H2 Cl2)'
_chemical_formula_sum            'C27 H34 Al Cl4 N2 Na O8'
_chemical_formula_weight         706.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                66.034(5)
_cell_angle_beta                 84.098(4)
_cell_angle_gamma                69.361(5)
_cell_formula_units_Z            2
_cell_length_a                   10.7960(5)
_cell_length_b                   11.9409(8)
_cell_length_c                   14.6196(7)
_cell_measurement_reflns_used    4582
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      76.2360
_cell_measurement_theta_min      3.3100
_cell_volume                     1609.86(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.986
_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     13.00  51.00   1.00    1.00    --    0.00 -99.00-150.00   38
  2  \w     14.00  44.00   1.00    1.00    --    0.00 -77.00  30.00   30
  3  \w    -21.00   6.00   1.00    1.00    --    0.00 -77.00  30.00   27
  4  \w     -5.00  36.00   1.00    1.00    --    0.00  19.00-150.00   41
  5  \w     56.00  83.00   1.00    1.00    --    0.00  19.00-150.00   27
  6  \w    -81.00   0.00   1.00    3.00    --  -60.50  77.00  90.00   81
  7  \w     15.00  40.00   1.00    3.00    --  -60.50  77.00  90.00   25
  8  \w    121.00 158.00   1.00    3.00    --   60.50  77.00 -30.00   37
  9  \w     97.00 122.00   1.00    3.00    --   60.50 125.00-180.00   25
 10  \w    101.00 152.00   1.00    3.00    --   60.50 125.00 -90.00   51
 11  \w    101.00 152.00   1.00    3.00    --   60.50 125.00  90.00   51
 12  \w    101.00 139.00   1.00    3.00    --   60.50 125.00  30.00   38
 13  \w    -31.00 152.00   1.00    3.00    --   60.50   0.00  30.00  183
 14  \w     27.00 112.00   1.00    3.00    --   60.50-125.00 -90.00   85
 15  \w    122.00 157.00   1.00    3.00    --   60.50  77.00 150.00   35
 16  \w     65.00  92.00   1.00    8.00    --  121.00 178.00   0.00   27
 17  \w     79.00 108.00   1.00    8.00    --  121.00-111.00 150.00   29
 18  \w     77.00 177.00   1.00    8.00    --  121.00  25.00 120.00  100
 19  \w     30.00  63.00   1.00    8.00    --  121.00 -37.00-120.00   33
 20  \w     29.00 108.00   1.00    8.00    --  121.00-111.00  90.00   79
 21  \w     45.00  70.00   1.00    8.00    --  121.00  25.00 120.00   25
 22  \w     30.00  85.00   1.00    8.00    --  121.00 -77.00   0.00   55
 23  \w     36.00 108.00   1.00    8.00    --  121.00-111.00   0.00   72
 24  \w     37.00  64.00   1.00    8.00    --  121.00 -37.00 -30.00   27
 25  \w     34.00  64.00   1.00    8.00    --  121.00 -37.00  90.00   30
 26  \w    108.00 178.00   1.00    8.00    --  121.00 111.00 -60.00   70
 27  \w     24.00 107.00   1.00    8.00    --  121.00 -91.00-150.00   83
 28  \w     62.00  92.00   1.00    8.00    --  121.00 -63.00  90.00   30
 29  \w     80.00 108.00   1.00    8.00    --  121.00-111.00-150.00   28
 30  \w     35.00 107.00   1.00    8.00    --  121.00-111.00 -60.00   72
 31  \w     30.00  55.00   1.00    8.00    --  121.00 -37.00 -90.00   25
 32  \w     81.00 178.00   1.00    8.00    --  121.00  50.00   0.00   97
 33  \w     40.00  80.00   1.00    8.00    --  121.00 -63.00-150.00   40
 34  \w     32.00  60.00   1.00    8.00    --  121.00 -37.00-150.00   28
 35  \w     35.00  78.00   1.00    8.00    --  121.00 -50.00  60.00   43
 36  \w     41.00  66.00   1.00    8.00    --  121.00 -50.00 120.00   25
 37  \w     56.00  87.00   1.00    8.00    --  121.00-111.00 -30.00   31
 38  \w     24.00  54.00   1.00    8.00    --  121.00 -91.00  60.00   30
 39  \w     82.00 107.00   1.00    8.00    --  121.00 -91.00  60.00   25
 40  \w     83.00 108.00   1.00    8.00    --  121.00-111.00  60.00   25
 41  \w     48.00  75.00   1.00    8.00    --  121.00  25.00-120.00   27
 42  \w    119.00 157.00   1.00    8.00    --  121.00  25.00-120.00   38
 43  \w     98.00 126.00   1.00    8.00    --  121.00 -77.00   0.00   28
;
_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      0.0104115000
_diffrn_orient_matrix_UB_12      -0.1381687000
_diffrn_orient_matrix_UB_13      0.0142178000
_diffrn_orient_matrix_UB_21      0.1087122000
_diffrn_orient_matrix_UB_22      -0.0010036000
_diffrn_orient_matrix_UB_23      -0.0769710000
_diffrn_orient_matrix_UB_31      0.1066597000
_diffrn_orient_matrix_UB_32      -0.0589934000
_diffrn_orient_matrix_UB_33      0.0848618000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12886
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.512
_diffrn_reflns_theta_min         3.312
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.168
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         6670
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0619P)^2^+0.3016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1210
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5365
_reflns_number_total             6670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c04020_si_002.cif
_cod_data_source_block           013rwfk20
_cod_database_code               4519050
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C25H33Al1N2Na1O8
_shelx_estimated_absorpt_t_max   0.812
_shelx_estimated_absorpt_t_min   0.534
_reflns_odcompleteness_completeness 99.71
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2S-C1S \\sim Cl3S-C1S
 with sigma of 0.02
3. Others
 Sof(H1SC)=Sof(H1SD)=Sof(Cl3S)=1-FVAR(1)
 Sof(Cl2S)=Sof(H1SA)=Sof(H1SB)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C13(H13A,H13B), C2S(H2SA,H2SB), C1S(H1SA,H1SB), C1S(H1SC,H1SD)
4.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C8(H8), C17(H17), C16(H16), C18(H18), C3(H3), C4(H4), C5(H5)
4.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C21(H21A,H21B,H21C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              52846
_shelx_hkl_checksum              98278
_ins_header
;
TITL 013RWFK20 in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  10.796037  11.940873  14.619565  66.0335  84.0984  69.3612
ZERR    3.00   0.000511   0.000807   0.000691   0.0054   0.0039   0.0052
LATT  1
SFAC C H N O Na Al
UNIT 75.00 99.00 6.00 24.00 3.00 3.00
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id 013RWFK20
_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 1.220
_oxdiff_exptl_absorpt_empirical_full_min 0.856