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_1568885
_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         'C52 H70 Al O2 P, C7 H8'
_chemical_formula_sum            'C59 H78 Al O2 P'
_chemical_formula_weight         877.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 103.1110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8537(3)
_cell_length_b                   15.5489(2)
_cell_length_c                   18.2578(3)
_cell_measurement_reflns_used    42128
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      1.00000
_cell_measurement_theta_min      0.86517
_cell_volume                     5212.83(14)
_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 0.950
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            60880
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.931
_diffrn_reflns_theta_min         2.406
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  0.8736
_exptl_absorpt_correction_T_min  0.7561
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         8966
_refine_ls_number_restraints     576
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0700P)^2^+5.8759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1426
_refine_ls_wR_factor_ref         0.1442
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8438
_reflns_number_total             8966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py00301a2.cif
_cod_data_source_block           czk-210803
_cod_depositor_comments
'Adding full bibliography for 1568884--1568888.cif.'
_cod_database_code               1568885
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.756
_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
 C53, C54, C55, C56, C57, C58, C59, C53A, C54A, C55A, C56A, C57A, C58A, C59A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C53A
\\sim C54A \\sim C55A \\sim C56A \\sim C57A \\sim C58A \\sim C59A: within 14A
with sigma of 0.02 and sigma for terminal atoms of 0.02
4. Others
 Sof(C53A)=Sof(H53A)=Sof(C54A)=Sof(H54A)=Sof(C55A)=Sof(H55A)=Sof(C56A)=
 Sof(H56A)=Sof(C57A)=Sof(H57A)=Sof(C58A)=Sof(C59A)=Sof(H59D)=Sof(H59E)=
 Sof(H59F)=1-FVAR(1)
 Sof(C53)=Sof(H53)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56)=
 Sof(C57)=Sof(H57)=Sof(C58)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
5.c Me refined with riding coordinates:
 C59(H59A,H59B,H59C), C59A(H59D,H59E,H59F)
5.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C29(H29),
  C32(H32), C44(H44), C47(H47), C53(H53), C54(H54), C55(H55), C56(H56),
 C57(H57), C53A(H53A), C54A(H54A), C55A(H55A), C56A(H56A), C57A(H57A)
5.e Fitted hexagon refined as free rotating group:
 C53(C54,C55,C56,C57,C58), C53A(C54A,C55A,C56A,C57A,C58A)
5.f Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C46(H46A,H46B,H46C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C52(H52A,H52B,H52C)
;
_shelx_res_checksum              63456
_olex2_submission_special_instructions 'No special instructions were received'