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_1568888
_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, 0.75(C6 H6), 0.25(C6)'
_chemical_formula_sum            'C63 H82.5 Al O4 P'
_chemical_formula_weight         961.73
_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   mixed
_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                67.9540(10)
_cell_angle_beta                 89.1970(10)
_cell_angle_gamma                74.8020(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6448(2)
_cell_length_b                   15.3492(2)
_cell_length_c                   16.4061(2)
_cell_measurement_reflns_used    54913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.0320
_cell_measurement_theta_min      2.8310
_cell_volume                     2835.47(7)
_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_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            66703
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.981
_diffrn_reflns_theta_min         2.919
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_T_max  0.8375
_exptl_absorpt_correction_T_min  0.8375
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1041
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.00054(9)
_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   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         10645
_refine_ls_number_restraints     565
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0463P)^2^+1.1566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10293
_reflns_number_total             10645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py00301a2.cif
_cod_data_source_block           czk-221220
_cod_depositor_comments
'Adding full bibliography for 1568884--1568888.cif.'
_cod_original_formula_sum        'C63 H82.50 Al O4 P'
_cod_database_code               1568888
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.837
_shelx_estimated_absorpt_t_min   0.837
_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. Restrained distances
 C4-C5 = C5-C6 = C4-C5A = C5A-C6A
 1.5 with sigma of 0.03
 C4-H4
 0.99 with sigma of 0.02
3. Rigid bond restraints
 C61, C62, C63, C64, C65, C66, C61A, C62A, C63A, C64A, C65A, C66A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C61B, C62B, C63B, C64B, C65B, C66B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5, C6, C5A, C6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Uiso/Uaniso restraints and constraints
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C61A \\sim C62A
\\sim C63A \\sim C64A \\sim C65A \\sim C66A: within 12A with sigma of 0.015 and
sigma for terminal atoms of 0.015
C61B \\sim C62B \\sim C63B \\sim C64B \\sim C65B \\sim C66B: within 6A with
sigma of 0.015 and sigma for terminal atoms of 0.015
C5 \\sim C6 \\sim C5A \\sim C6A: within 4A with sigma of 0.01 and sigma for
terminal atoms of 0.01
5. Others
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=1-FVAR(1)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=FVAR(1)
 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) H66(0.25) C61A(0.5)
 H61A(0.5) C62A(0.5) H62A(0.5) C63A(0.5) H63A(0.5) C64A(0.5) H64A(0.5)
 C65A(0.5) H65A(0.5) C66A(0.5) H66A(0.5) C61B(0.25) C62B(0.25) C63B(0.25)
 C64B(0.25) C65B(0.25) C66B(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C5A(H5AA,H5AB)
6.b Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C6A(H6AA,H6AB,H6AC)
6.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C34(H34), C37(H37), C49(H49), C52(H52), C61(H61), C62(H62), C63(H63),
 C64(H64), C65(H65), C66(H66), C61A(H61A), C62A(H62A), C63A(H63A), C64A(H64A),
 C65A(H65A), C66A(H66A)
6.d Fitted hexagon refined as free rotating group:
 C61(C62,C63,C64,C65,C66), C61A(C62A,C63A,C64A,C65A,C66A), C61B(C62B,C63B,C64B,
 C65B,C66B)
6.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C27(H27A,H27B,H27C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C51(H51A,H51B,H51C), C55(H55A,H55B,H55C),
 C56(H56A,H56B,H56C), C57(H57A,H57B,H57C)
;
_shelx_res_checksum              23075
_olex2_submission_special_instructions 'No special instructions were received'