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_4519054
_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         'C74 H76 Al2 K2 N4 O17'
_chemical_formula_sum            'C74 H76 Al2 K2 N4 O17'
_chemical_formula_weight         1425.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.699(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0779(2)
_cell_length_b                   30.1479(4)
_cell_length_c                   17.5249(3)
_cell_measurement_reflns_used    12650
_cell_measurement_temperature    150.00(13)
_cell_measurement_theta_max      75.7420
_cell_measurement_theta_min      3.0970
_cell_volume                     7237.5(2)
_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      150.00(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_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    -39.00  12.00   1.00    8.00    --  -42.66  57.00-120.00   51
  2  \w      0.00  27.00   1.00    8.00    --  -42.66  19.00-150.00   27
  3  \w     -1.00  31.00   1.00    8.00    --  -42.66  19.00 -30.00   32
  4  \w     -3.00  35.00   1.00    8.00    --  -42.66  19.00 120.00   38
  5  \w     -5.00  30.00   1.00    8.00    --  -42.66  19.00-180.00   35
  6  \w     76.00 129.00   1.00    8.00    --   42.66 178.00 -90.00   53
  7  \w     92.00 164.00   1.00   30.00    --  111.00  45.00 -30.00   72
  8  \w     60.00 106.00   1.00   30.00    --  111.00 -95.00 120.00   46
  9  \w     40.00  69.00   1.00   30.00    --  111.00 -45.00-150.00   29
 10  \w     42.00  68.00   1.00   30.00    --  111.00 -45.00 -60.00   26
 11  \w     55.00  81.00   1.00   30.00    --  111.00 -61.00-180.00   26
 12  \w     41.00  71.00   1.00   30.00    --  111.00 -45.00  30.00   30
 13  \w    150.00 176.00   1.00   30.00    --  111.00 125.00  30.00   26
 14  \w     33.00  73.00   1.00   30.00    --  111.00 -95.00-150.00   40
 15  \w    106.00 153.00   1.00   30.00    --  111.00 125.00-120.00   47
 16  \w     75.00 101.00   1.00   30.00    --  111.00 -95.00-150.00   26
 17  \w     40.00  70.00   1.00   30.00    --  111.00 -45.00 -90.00   30
 18  \w     87.00 177.00   1.00   30.00    --  111.00  45.00 -60.00   90
 19  \w     48.00 107.00   1.00   30.00    --  111.00-120.00 131.00   59
 20  \w     58.00  91.00   1.00   30.00    --  111.00 -61.00 120.00   33
 21  \w     39.00  84.00   1.00   30.00    --  111.00 -95.00 150.00   45
 22  \w     90.00 167.00   1.00   30.00    --  111.00  45.00  60.00   77
 23  \w     83.00 109.00   1.00   30.00    --  111.00-114.00-155.61   26
 24  \w     42.00  67.00   1.00   30.00    --  111.00-114.00-155.61   25
 25  \w    -21.00 -19.00   1.00    8.00    --  -42.66  38.00  30.00    2
;
_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      -0.0052235000
_diffrn_orient_matrix_UB_12      0.0504429000
_diffrn_orient_matrix_UB_13      0.0116686000
_diffrn_orient_matrix_UB_21      0.0567223000
_diffrn_orient_matrix_UB_22      -0.0056478000
_diffrn_orient_matrix_UB_23      0.0956786000
_diffrn_orient_matrix_UB_31      0.0969631000
_diffrn_orient_matrix_UB_32      0.0060150000
_diffrn_orient_matrix_UB_33      -0.0084180000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44644
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.190
_diffrn_reflns_theta_min         3.139
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.979
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77784
_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            'dull yellow'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       needle
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     900
_refine_ls_number_reflns         14927
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+1.0925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1144
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11897
_reflns_number_total             14927
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c04020_si_002.cif
_cod_data_source_block           021rwfk21
_cod_database_code               4519054
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C100H100Al1K1N4O10
_reflns_odcompleteness_completeness 99.56
_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 Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C44(H44A,H44B), C48(H48A,H48B), C13(H13A,H13B), C73(H73A,H73B),
 C72(H72A,H72B), C74(H74A,H74B), C71(H71A,H71B)
2.b Aromatic/amide H refined with riding coordinates:
 C49(H49), C70(H70), C24(H24), C43(H43), C14(H14), C8(H8), C38(H38), C31(H31),
 C51(H51), C53(H53), C28(H28), C25(H25), C66(H66), C52(H52), C26(H26), C68(H68),
  C59(H59), C39(H39), C32(H32), C16(H16), C67(H67), C69(H69), C40(H40),
 C27(H27), C5(H5), C35(H35), C17(H17), C18(H18), C33(H33), C63(H63), C34(H34),
 C3(H3), C4(H4), C61(H61), C60(H60), C62(H62)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C47(H47A,H47B,H47C), C36(H36A,H36B,H36C), C12(H12A,H12B,
 H12C), C56(H56A,H56B,H56C), C46(H46A,H46B,H46C), C21(H21A,H21B,H21C), C1(H1A,
 H1B,H1C)
;
_shelx_res_checksum              14676
_shelx_hkl_checksum              86104
_shelx_fab_checksum              24545
_ins_header
;
TITL 021RWFK21 in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  15.077907  30.147922  17.524862  90.0000 114.6993  90.0000
ZERR    7.00   0.000209   0.000395   0.000256   0.0000   0.0018   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H N O Al K
UNIT 700.00 700.00 28.00 70.00 7.00 7.00
TREF
HKLF 4
END
;
_olex2_date_sample_data_collection 2021-06-04
_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 1.395
_oxdiff_exptl_absorpt_empirical_full_min 0.633