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_4519051
_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 K2 N4 O16, C H Cl3'
_chemical_formula_sum            'C51 H61 Al2 Cl3 K2 N4 O16'
_chemical_formula_weight         1224.54
_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             2021-07-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                65.273(5)
_cell_angle_beta                 82.478(4)
_cell_angle_gamma                76.607(5)
_cell_formula_units_Z            2
_cell_length_a                   12.4551(6)
_cell_length_b                   15.8089(10)
_cell_length_c                   16.1748(8)
_cell_measurement_reflns_used    5456
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      27.6510
_cell_measurement_theta_min      1.9880
_cell_volume                     2812.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (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 1.000
_diffrn_measured_fraction_theta_max 0.874
_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    -19.00 105.00   1.00   67.50    --   21.82  77.00 150.00  124
  2  \w    -11.00 104.00   1.00   67.50    --   21.82  77.00  30.00  115
  3  \w    -14.00 105.00   1.00   67.50    --   21.82  77.00 -90.00  119
;
_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      0.0158839000
_diffrn_orient_matrix_UB_12      0.0390501000
_diffrn_orient_matrix_UB_13      0.0026582000
_diffrn_orient_matrix_UB_21      -0.0520469000
_diffrn_orient_matrix_UB_22      0.0287483000
_diffrn_orient_matrix_UB_23      -0.0160607000
_diffrn_orient_matrix_UB_31      -0.0216998000
_diffrn_orient_matrix_UB_32      -0.0136562000
_diffrn_orient_matrix_UB_33      0.0454895000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0953
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21284
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.663
_diffrn_reflns_theta_min         1.682
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.414
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.074
_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     715
_refine_ls_number_reflns         13911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0609
_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^)+(0.0326P)^2^+0.5347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1294
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8926
_reflns_number_total             13911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c04020_si_002.cif
_cod_data_source_block           063ap20
_cod_database_code               4519051
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H40 O8 N2 Co1 K1'
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.935
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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), C33(H33), C8(H8), C5(H5), C30(H30), C16(H16), C3(H3), C28(H28),
 C39(H39), C17(H17), C18(H18), C41(H41), C29(H29), C4(H4), C43(H43), C42(H42)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C1(H1A,H1B,H1C), C37(H37A,H37B,H37C), C26(H26A,H26B,
 H26C), C48(H48A,H48B,H48C), C11(H11A,H11B,H11C), C25(H25A,H25B,H25C), C36(H36A,
 H36B,H36C), C50(H50A,H50B,H50C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C),
 C46(H46A,H46B,H46C)
;
_shelx_res_checksum              78923
_shelx_hkl_checksum              40977
_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 1.236
_oxdiff_exptl_absorpt_empirical_full_min 0.897