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_1568886
_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         '2(C51 H68 Al O2 P), 2(C7 H8)'
_chemical_formula_sum            'C116 H152 Al2 O4 P2'
_chemical_formula_weight         1726.27
_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                73.892(2)
_cell_angle_beta                 88.976(2)
_cell_angle_gamma                88.672(2)
_cell_formula_units_Z            2
_cell_length_a                   15.9438(4)
_cell_length_b                   17.9944(3)
_cell_length_c                   18.5158(4)
_cell_measurement_reflns_used    32210
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      58.8180
_cell_measurement_theta_min      2.4990
_cell_volume                     5101.9(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 0.775
_diffrn_measured_fraction_theta_max 0.981
_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    -76.00 -48.00   1.00    0.32    --    0.86 178.00   0.00   28
  2  \w    -81.00 -56.00   1.00    0.32    --    0.86 178.00  90.00   25
  3  \w     11.00  76.00   1.00    0.32    --    0.86  57.00-150.00   65
  4  \w    -21.00  10.00   1.00    0.32    --    0.86  57.00-150.00   31
  5  \w    -28.00  43.00   1.00    0.32    --    0.86  86.00 128.00   71
  6  \w     93.00 151.00   1.00    1.28    --   75.81 125.00  90.00   58
  7  \w    107.00 133.00   1.00    1.28    --   75.81  86.00 128.00   26
  8  \w     35.00 107.00   1.00    1.28    --   75.81 -86.00  10.00   72
  9  \w     33.00 101.00   1.00    1.28    --   75.81-125.00  30.00   68
 10  \w     56.00 116.00   1.00    1.28    --   75.81-125.00  90.00   60
 11  \w     48.00 102.00   1.00    1.28    --   75.81-125.00 -30.00   54
 12  \w     32.00 117.00   1.00    1.28    --   75.81-125.00-150.00   85
 13  \w     45.00 103.00   1.00    1.28    --   75.81 -99.00-150.00   58
 14  \w      1.00  37.00   1.00    1.28    --   75.81 -99.00-150.00   36
 15  \w      1.00  31.00   1.00    0.32    --    0.86 -99.00 -90.00   30
 16  \w    -20.00  31.00   1.00    0.32    --    0.86 -86.00  10.00   51
 17  \w      6.00  58.00   1.00    1.28    --   75.81 -57.00-120.00   52
 18  \w      2.00  55.00   1.00    1.28    --   75.81 -57.00-150.00   53
 19  \w      7.00  34.00   1.00    1.28    --   75.81 -57.00-180.00   27
 20  \w     -4.00  26.00   1.00    1.28    --   75.81 -19.00-180.00   30
 21  \w     -6.00  19.00   1.00    1.28    --   75.81 -19.00-150.00   25
 22  \w     -6.00  26.00   1.00    1.28    --   75.81 -19.00 -90.00   32
 23  \w     -2.00  23.00   1.00    1.28    --   75.81 -19.00  30.00   25
 24  \w     -6.00  26.00   1.00    1.28    --   75.81 -19.00  60.00   32
 25  \w     -6.00  25.00   1.00    1.28    --   75.81 -19.00  90.00   31
 26  \w     -6.00  25.00   1.00    1.28    --   75.81 -19.00 120.00   31
 27  \w   -143.00-111.00   1.00    1.28    --  -74.09 -86.00  10.00   32
 28  \w   -108.00 -83.00   1.00    1.28    --  -74.09 -86.00  10.00   25
 29  \w    -41.00  -2.00   1.00    1.28    --  -74.09  37.00 120.00   39
 30  \w    -38.00  -8.00   1.00    1.28    --  -74.09  37.00  90.00   30
 31  \w    -40.00   5.00   1.00    1.28    --  -74.09  37.00  60.00   45
 32  \w    -25.00   6.00   1.00    1.28    --  -74.09  19.00  60.00   31
 33  \w    -26.00   6.00   1.00    1.28    --  -74.09  19.00  30.00   32
 34  \w    -20.00   6.00   1.00    1.28    --  -74.09  19.00 -30.00   26
 35  \w    -29.00   0.00   1.00    1.28    --  -74.09  37.00 -60.00   29
 36  \w    -90.00 -42.00   1.00    1.28    --  -74.09 125.00  90.00   48
 37  \w    -68.00 -42.00   1.00    1.28    --  -74.09  86.00 128.00   26
 38  \w    -59.00 -11.00   1.00    1.28    --  -74.09 125.00  30.00   48
;
_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      0.0916813000
_diffrn_orient_matrix_UB_12      -0.0029981000
_diffrn_orient_matrix_UB_13      -0.0269217000
_diffrn_orient_matrix_UB_21      -0.0203114000
_diffrn_orient_matrix_UB_22      0.0641753000
_diffrn_orient_matrix_UB_23      -0.0723649000
_diffrn_orient_matrix_UB_31      0.0229042000
_diffrn_orient_matrix_UB_32      0.0617766000
_diffrn_orient_matrix_UB_33      0.0392375000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.775
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            46473
_diffrn_reflns_point_group_measured_fraction_full 0.775
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         58.778
_diffrn_reflns_theta_min         2.484
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.939
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87688
_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    1.124
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.00027(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1191
_refine_ls_number_reflns         14312
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0478P)^2^+3.4668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13228
_reflns_number_total             14312
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py00301a2.cif
_cod_data_source_block           czk-210721
_cod_depositor_comments
'Adding full bibliography for 1568884--1568888.cif.'
_cod_database_code               1568886
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Si C N B'
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.834
_diffrn_oxdiff_digest_frames
;
01c51cb02aafeda9ef748c30c3a8a41ab3015679740
;
_diffrn_oxdiff_digest_hkl
;
01a8a6fc89ed4261ebf7c286a61a6343040116
;
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     55.92
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C110, C111, C112, C113, C114, C115, C116
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C7A, C1A, C2A, C3A, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C110 \\sim C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116: within
7A with sigma of 0.015 and sigma for terminal atoms of 0.015
C7A \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A: within 2A with
sigma of 0.015 and sigma for terminal atoms of 0.015
4. Others
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=
 Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=1-FVAR(1)
 Sof(C110)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C111)=Sof(C112)=Sof(H112)=
 Sof(C113)=Sof(H113)=Sof(C114)=Sof(H114)=Sof(C115)=Sof(H115)=Sof(C116)=
 Sof(H116)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C53(H53)
5.b Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C21(H21A,H21B,H21C)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C24(H24),
  C26(H26), C39(H39), C41(H41), C55(H55), C56(H56), C57(H57), C58(H58),
 C59(H59), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C67(H67), C68(H68),
  C69(H69), C70(H70), C71(H71), C75(H75), C77(H77), C90(H90), C92(H92),
 C105(H105), C106(H106), C107(H107), C108(H108), C109(H109), C112(H112),
 C113(H113), C114(H114), C115(H115), C116(H116), C1A(H1A), C2A(H2AA), C3A(H3A),
 C4A(H4A), C5A(H5A)
5.d Fitted hexagon refined as free rotating group:
 C111(C112,C113,C114,C115,C116), C1A(C2A,C3A,C4A,C5A,C6A)
5.e Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C43(H43A,
 H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C72(H72A,H72B,H72C), C79(H79A,H79B,H79C), C81(H81A,H81B,H81C), C82(H82A,
 H82B,H82C), C83(H83A,H83B,H83C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C),
 C87(H87A,H87B,H87C), C94(H94A,H94B,H94C), C96(H96A,H96B,H96C), C97(H97A,H97B,
 H97C), C98(H98A,H98B,H98C), C100(H10A,H10B,H10C), C101(H10D,H10E,H10F),
 C102(H10G,H10H,H10I), C103(H10J,H10K,H10L), C110(H11A,H11B,H11C), C7A(H7AA,
 H7AB,H7AC)
;
_shelx_res_checksum              4095
_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 1.281
_oxdiff_exptl_absorpt_empirical_full_min 0.748