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_4519052
_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         'C50 H60 Al2 N4 O16 Rb2, C H Cl3'
_chemical_formula_sum            'C51 H61 Al2 Cl3 N4 O16 Rb2'
_chemical_formula_weight         1317.28
_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             2021-03-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                64.372(3)
_cell_angle_beta                 82.396(2)
_cell_angle_gamma                76.638(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5460(3)
_cell_length_b                   15.7343(4)
_cell_length_c                   16.4513(5)
_cell_measurement_reflns_used    18002
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      76.5160
_cell_measurement_theta_min      2.9770
_cell_volume                     2846.84(15)
_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      149.99(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     43.00  94.00   1.00    1.00    --    0.00  19.00  90.00   51
  2  \w    -15.00  39.00   1.00    1.00    --    0.00 -77.00 -90.00   54
  3  \w     -7.00  35.00   1.00    1.00    --    0.00 -77.00 120.00   42
  4  \w     -3.00  30.00   1.00    1.00    --    0.00  19.00  90.00   33
  5  \w   -153.00  29.00   1.00    2.00    --  -60.50 -15.00  60.00  182
  6  \w    -87.00 -32.00   1.00    2.00    --  -60.50 125.00  60.00   55
  7  \w      1.00  31.00   1.00    2.00    --  -60.50  30.00 -60.00   30
  8  \w     97.00 143.00   1.00    2.00    --   60.50 125.00  30.00   46
  9  \w     97.00 148.00   1.00    2.00    --   60.50 125.00 150.00   51
 10  \w    107.00 155.00   1.00    2.00    --   60.50  77.00 120.00   48
 11  \w    103.00 133.00   1.00    2.00    --   60.50 125.00-180.00   30
 12  \w    114.00 150.00   1.00    2.00    --   60.50 125.00 -60.00   36
 13  \w     29.00 111.00   1.00    2.00    --   60.50-125.00   0.00   82
 14  \w     99.00 151.00   1.00    2.00    --   60.50 135.00 -20.00   52
 15  \w    101.00 126.00   1.00    2.00    --   60.50 125.00 -90.00   25
 16  \w     47.00  89.00   1.00    3.00    --  121.00 -91.00-150.00   42
 17  \w     60.00 108.00   1.00    3.00    --  121.00-111.00  30.00   48
 18  \w     31.00  64.00   1.00    3.00    --  121.00 -37.00 120.00   33
 19  \w     32.00 106.00   1.00    3.00    --  121.00-111.00  90.00   74
 20  \w     68.00 108.00   1.00    3.00    --  121.00-111.00  60.00   40
 21  \w     48.00  85.00   1.00    3.00    --  121.00 -63.00 -90.00   37
 22  \w     28.00  60.00   1.00    3.00    --  121.00 -77.00  30.00   32
 23  \w     78.00 171.00   1.00    3.00    --  121.00  63.00 120.00   93
 24  \w     30.00  57.00   1.00    3.00    --  121.00 -37.00-150.00   27
 25  \w     74.00 108.00   1.00    3.00    --  121.00-111.00-150.00   34
 26  \w     39.00 108.00   1.00    3.00    --  121.00-111.00 -60.00   69
 27  \w     29.00  59.00   1.00    3.00    --  121.00-111.00 -30.00   30
 28  \w     83.00 108.00   1.00    3.00    --  121.00-111.00 -30.00   25
 29  \w     34.00  60.00   1.00    3.00    --  121.00 -50.00  60.00   26
 30  \w    116.00 166.00   1.00    3.00    --  121.00  77.00-150.00   50
 31  \w    128.00 154.00   1.00    3.00    --  121.00  37.00 120.00   26
 32  \w    106.00 137.00   1.00    3.00    --  121.00  77.00  90.00   31
 33  \w    119.00 153.00   1.00    3.00    --  121.00 111.00 150.00   34
 34  \w     31.00  64.00   1.00    3.00    --  121.00 -37.00-180.00   33
 35  \w     55.00 107.00   1.00    3.00    --  121.00-111.00-180.00   52
 36  \w     72.00 107.00   1.00    3.00    --  121.00-111.00 150.00   35
 37  \w    151.00 177.00   1.00    3.00    --  121.00 111.00 -60.00   26
 38  \w    144.00 169.00   1.00    3.00    --  121.00  77.00  90.00   25
 39  \w    104.00 169.00   1.00    3.00    --  121.00  77.00 -30.00   65
 40  \w    110.00 136.00   1.00    3.00    --  121.00 111.00 -60.00   26
 41  \w     39.00  64.00   1.00    3.00    --  121.00 -77.00-120.00   25
 42  \w    100.00 125.00   1.00    3.00    --  121.00 -77.00-120.00   25
 43  \w     39.00  72.00   1.00    3.00    --  121.00 -50.00 -60.00   33
 44  \w     43.00  69.00   1.00    3.00    --  121.00 -50.00  90.00   26
 45  \w    103.00 165.00   1.00    3.00    --  121.00  77.00  60.00   62
 46  \w     65.00 104.00   1.00    3.00    --  121.00-111.00 -90.00   39
 47  \w     95.00 153.00   1.00    3.00    --  121.00  37.00  30.00   58
 48  \w     89.00 119.00   1.00    3.00    --  121.00 -77.00  30.00   30
 49  \w    -21.00  19.00   1.00    1.00    --    0.00  37.00 -30.00   40
 50  \w    -41.00  -1.00   1.00    1.00    --    0.00  77.00  60.00   40
 51  \w     13.00  40.00   1.00    1.00    --    0.00 -99.00-180.00   27
 52  \w      0.00  35.00   1.00    1.00    --    0.00  77.00  60.00   35
 53  \w     28.00  81.00   1.00    1.00    --    0.00  37.00 -30.00   53
 54  \w    -19.00   7.00   1.00    2.00    --   38.00 110.00 100.29   26
 55  \w     -7.00  18.00   1.00    2.00    --   42.00  94.00 155.17   25
 56  \w      4.00  29.00   1.00    2.00    --   50.00  88.00-121.46   25
 57  \w      4.00  30.00   1.00    2.00    --   50.00  89.00 -39.75   26
 58  \w     16.00  42.00   1.00    2.00    --   60.50  81.00  93.70   26
 59  \w     16.00  42.00   1.00    2.00    --   60.50  82.00  22.66   26
 60  \w     16.00  41.00   1.00    2.00    --   60.50  82.00  -6.34   25
 61  \w     16.00  41.00   1.00    2.00    --   60.50  82.00-150.75   25
 62  \w     16.00  41.00   1.00    2.00    --   60.50  82.00 152.89   25
 63  \w     16.00  41.00   1.00    2.00    --   60.50  81.00 -81.61   25
 64  \w     24.00  51.00   1.00    2.00    --   66.00  74.00  71.26   27
 65  \w     23.00 150.00   1.00    2.00    --   66.00  71.00-108.55  127
;
_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      0.0223989000
_diffrn_orient_matrix_UB_12      0.1011763000
_diffrn_orient_matrix_UB_13      -0.0613118000
_diffrn_orient_matrix_UB_21      0.0116239000
_diffrn_orient_matrix_UB_22      0.0164235000
_diffrn_orient_matrix_UB_23      0.0839183000
_diffrn_orient_matrix_UB_31      0.1237489000
_diffrn_orient_matrix_UB_32      -0.0418377000
_diffrn_orient_matrix_UB_33      -0.0006980000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30073
_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         76.599
_diffrn_reflns_theta_min         2.981
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.422
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73130
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       block
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         11825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0477P)^2^+0.6245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0884
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10423
_reflns_number_total             11825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c04020_si_002.cif
_cod_data_source_block           014rwfk20
_cod_database_code               4519052
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C100H100Al1N2O8Rb1
_shelx_estimated_absorpt_t_max   0.612
_shelx_estimated_absorpt_t_min   0.303
_reflns_odcompleteness_completeness 99.79
_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.a Ternary CH refined with riding coordinates:
 C1S(H1S)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C13(H13A,H13B), C38(H38A,H38B), C34(H34A,H34B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C39(H39), C8(H8), C41(H41), C33(H33), C16(H16), C5(H5), C3(H3),
 C18(H18), C30(H30), C4(H4), C43(H43), C17(H17), C42(H42), C29(H29), C28(H28)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C25(H25A,H25B,H25C), C48(H48A,H48B,H48C), C11(H11A,H11B,
 H11C), C36(H36A,H36B,H36C), C21(H21A,H21B,H21C), C46(H46A,H46B,H46C), C1(H1A,
 H1B,H1C), C23(H23A,H23B,H23C), C37(H37A,H37B,H37C), C26(H26A,H26B,H26C),
 C50(H50A,H50B,H50C)
;
_shelx_res_checksum              41236
_shelx_hkl_checksum              36951
_ins_header
;
TITL 014RWFK20 in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  12.545975  15.734270  16.451350  64.3717  82.3965  76.6383
ZERR    2.00   0.000257   0.000439   0.000498   0.0029   0.0021   0.0020
LATT  1
SFAC C H N O Al Rb
UNIT 200.00 200.00 4.00 16.00 2.00 2.00
REM  CrysAlisPro recorded range (K): Min=149.9; max=150.0; aver:150.0
TEMP -123
TREF
HKLF 4
END
;
_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 1.270
_oxdiff_exptl_absorpt_empirical_full_min 0.764