Phosphonium ylide/organoaluminum-based Lewis pairs for the highly efficient living/controlled polymerization of alkyl (meth)acrylates
Chen, Zhikang; Zhao, Wuchao; Liu, Conglei; Jiang, Liuying; Fu, Gang; Zhang, Yuetao; Zhu, Hongping; Polymer Chemistry 14 (2023) 2344–2354; doi:10.1039/D3PY00301A

data_1568887
_publ_section_title
;
 Phosphonium ylide/organoaluminum-based Lewis pairs for the highly
 efficient living/controlled polymerization of alkyl (meth)acrylates
;
_journal_issue                   19
_journal_name_full               'Polymer Chemistry'
_journal_page_first              2344
_journal_page_last               2354
_journal_paper_doi               10.1039/D3PY00301A
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C57 H78 Al O4 P, 0.5(C7 H8)'
_chemical_formula_sum            'C60.5 H82 Al O4 P'
_chemical_formula_weight         931.21
_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
_audit_creation_date             2022-12-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-12-23 deposited with the CCDC.	2023-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                109.495(4)
_cell_angle_beta                 92.100(3)
_cell_angle_gamma                107.404(3)
_cell_formula_units_Z            2
_cell_length_a                   12.9446(4)
_cell_length_b                   14.8659(6)
_cell_length_c                   17.9817(7)
_cell_measurement_reflns_used    8279
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      58.3110
_cell_measurement_theta_min      2.6510
_cell_volume                     3076.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.772
_diffrn_measured_fraction_theta_max 0.973
_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    -26.00   2.00   1.00    8.20    --    0.86 110.00 -16.00   28
  2  \w    -84.00 -39.00   1.00   10.50    --  -74.09 110.00 -16.00   45
  3  \w   -140.00-115.00   1.00   10.50    --  -74.09-110.00-111.00   25
  4  \w    100.00 127.00   1.00   10.50    --   75.81 110.00 -16.00   27
  5  \w     35.00 112.00   1.00   10.50    --   75.81-110.00-111.00   77
  6  \w     37.00  65.00   1.00    8.20    --    0.86  57.00-180.00   28
  7  \w    -79.00 -50.00   1.00    8.20    --    0.86 178.00 -60.00   29
  8  \w    -23.00  57.00   1.00    8.20    --    0.86  77.00  60.00   80
  9  \w    -75.00 -40.00   1.00    8.20    --    0.86 178.00 120.00   35
 10  \w    -22.00  35.00   1.00    8.20    --    0.86  57.00-180.00   57
 11  \w    -26.00   0.00   1.00   10.50    --  -74.09  19.00 -90.00   26
 12  \w    -41.00   3.00   1.00   10.50    --  -74.09  37.00  90.00   44
 13  \w    -70.00 -27.00   1.00   10.50    --  -74.09  77.00-180.00   43
 14  \w   -100.00 -73.00   1.00   10.50    --  -74.09  77.00-180.00   27
 15  \w    -79.00  -1.00   1.00   10.50    --  -74.09  77.00 -90.00   78
 16  \w    -65.00  -3.00   1.00   10.50    --  -74.09  57.00 -90.00   62
 17  \w    -34.00   1.00   1.00   10.50    --  -74.09  57.00   0.00   35
 18  \w    -49.00   1.00   1.00   10.50    --  -74.09  57.00 -30.00   50
 19  \w    -62.00 -35.00   1.00   10.50    --  -74.09  57.00   0.00   27
 20  \w    -30.00  -5.00   1.00   10.50    --  -74.09 110.00 -16.00   25
 21  \w   -154.00 -50.00   1.00   10.50    --  -74.09 -37.00 120.00  104
 22  \w     41.00  66.00   1.00   10.50    --   75.81 -57.00 -90.00   25
 23  \w     -3.00  26.00   1.00   10.50    --   75.81 -19.00 -60.00   29
 24  \w     -5.00  23.00   1.00   10.50    --   75.81 -19.00   0.00   28
 25  \w     -6.00  26.00   1.00   10.50    --   75.81 -19.00 -30.00   32
 26  \w     -5.00  20.00   1.00   10.50    --   75.81 -19.00  30.00   25
 27  \w     -5.00  26.00   1.00   10.50    --   75.81 -19.00 150.00   31
 28  \w     50.00 117.00   1.00   10.50    --   75.81-125.00  90.00   67
 29  \w     -6.00  26.00   1.00   10.50    --   75.81 -19.00-120.00   32
 30  \w     -6.00  20.00   1.00   10.50    --   75.81 -19.00-180.00   26
 31  \w     50.00 107.00   1.00   10.50    --   75.81-125.00 150.00   57
 32  \w      2.00  66.00   1.00   10.50    --   75.81 -57.00  60.00   64
 33  \w      9.00  61.00   1.00   10.50    --   75.81 -57.00 120.00   52
 34  \w     -6.00  19.00   1.00   10.50    --   75.81 -19.00 -90.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0592752000
_diffrn_orient_matrix_UB_12      0.0750650000
_diffrn_orient_matrix_UB_13      -0.0389491000
_diffrn_orient_matrix_UB_21      0.0240775000
_diffrn_orient_matrix_UB_22      0.0876763000
_diffrn_orient_matrix_UB_23      0.0809809000
_diffrn_orient_matrix_UB_31      0.1087590000
_diffrn_orient_matrix_UB_32      -0.0156602000
_diffrn_orient_matrix_UB_33      0.0194836000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.772
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25538
_diffrn_reflns_point_group_measured_fraction_full 0.772
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         58.852
_diffrn_reflns_theta_min         2.637
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.005
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1010
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         8588
_refine_ls_number_restraints     576
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.0969
_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^)+(0.1647P)^2^+4.0243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2643
_refine_ls_wR_factor_ref         0.2786
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7134
_reflns_number_total             8588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py00301a2.cif
_cod_data_source_block           czk-210720
_cod_depositor_comments
'Adding full bibliography for 1568884--1568888.cif.'
_cod_original_formula_sum        'C60.50 H82 Al O4 P'
_cod_database_code               1568887
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C H P O Al'
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.921
_diffrn_oxdiff_digest_frames
;
01589e7a2a45ac9d52ecb01c905c15c4e8000257ee0
;
_diffrn_oxdiff_digest_hkl
;
01906c031d782b85efc7452cde43dbb8ca63ca
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     55.92
_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. Rigid bond restraints
 C61, C62, C63, C64, C65, C66, C67, C68, C69, C70, C71, C72, C73, C74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Uiso/Uaniso restraints and constraints
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim
C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74: within 14A with sigma of
0.01 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C61(0.25) H61(0.25) C62(0.25) H62(0.25) C63(0.25) H63(0.25)
 C64(0.25) H64(0.25) C65(0.25) H65(0.25) C66(0.25) C67(0.25) H67A(0.25)
 H67B(0.25) H67C(0.25) C68(0.25) H68(0.25) C69(0.25) H69(0.25) C70(0.25)
 H70(0.25) C71(0.25) H71(0.25) C72(0.25) H72(0.25) C73(0.25) C74(0.25)
 H74A(0.25) H74B(0.25) H74C(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
5.b Me refined with riding coordinates:
 C16(H16A,H16B,H16C)
5.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C27(H27), C29(H29), C41(H41), C42(H42), C43(H43),
 C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C53(H53),
  C54(H54), C55(H55), C56(H56), C57(H57), C61(H61), C62(H62), C63(H63),
 C64(H64), C65(H65), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
5.d Fitted hexagon refined as free rotating group:
 C61(C62,C63,C64,C65,C66), C68(C69,C70,C71,C72,C73)
5.e Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C31(H31A,H31B,
 H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,
 H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C67(H67A,H67B,H67C),
 C74(H74A,H74B,H74C)
;
_shelx_res_checksum              38348
_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 1.644
_oxdiff_exptl_absorpt_empirical_full_min 0.604