Living polymerization of naturally renewable butyrolactone-based vinylidenes mediated by a frustrated Lewis pair
Bai, Yun; Wang, Huaiyu; He, Jianghua; Zhang, Yuetao; Polymer Chemistry 12 (2021) 5548–5555; doi:10.1039/D1PY00924A

data_1564526
_publ_section_title
;
 Living polymerization of naturally renewable butyrolactone-based
 vinylidenes mediated by a frustrated Lewis pair
;
_journal_issue                   38
_journal_name_full               'Polymer Chemistry'
_journal_page_first              5548
_journal_page_last               5555
_journal_paper_doi               10.1039/D1PY00924A
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C57 H97 Al N3 O4 P, C3 H3'
_chemical_formula_sum            'C60 H100 Al N3 O4 P'
_chemical_formula_weight         985.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-30 deposited with the CCDC.	2021-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.599(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.437(2)
_cell_length_b                   15.0322(18)
_cell_length_c                   20.796(2)
_cell_measurement_reflns_used    1498
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      17.669
_cell_measurement_theta_min      2.38
_cell_volume                     6073.8(11)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_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_temperature      273.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1361
_diffrn_reflns_av_unetI/netI     0.1909
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34143
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.414
_exptl_absorpt_coefficient_mu    0.104
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_description       block
_exptl_crystal_F_000             2164
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         12334
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.2091
_refine_ls_R_factor_gt           0.0794
_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^)+(0.0884P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.2213
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4882
_reflns_number_total             12334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1py00924a2.cif
_cod_data_source_block           test
_cod_depositor_comments          'Adding full bibliography for 1564526.cif.'
_cod_database_code               1564526
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.992
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-C4 = O2-C4A
 1.46 with sigma of 0.005
 C5A-C4A = C5-C4 = C4A-C3 = C4-C3
 1.54 with sigma of 0.005
 C9-C7 = C9A-C7 = C8-C7
 1.54 with sigma of 0.005
 C59-C58 = C60-C59
 1.39 with sigma of 0.005
 C5-C3 = C5A-C3
 2.52 with sigma of 0.005
 C8-C9 = C8-C9A
 2.52 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C5 \\sim C60 \\sim C58 \\sim C59: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C9A) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Sof(H3BC)=Sof(H3BD)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C4A)=Sof(H4A)=
 1-FVAR(1)
 Sof(H3AA)=Sof(H3AB)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(1)
 Sof(H7B)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(2)
 Sof(H7A)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C4(H4), C7(H7A), C7(H7B), C10(H10), C14(H14), C21(H21), C55(H55), C4A(H4A)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3AA,H3AB), C3(H3BC,H3BD), C6(H6A,H6B), C54(H54A,H54B)
5.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C28(H28), C41(H41), C43(H43), C58(H58), C59(H59), C60(H60)
5.d Idealised Me refined as rotating group:
 C5A(H5AA,H5AB,H5AC), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C),
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,
 H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C56(H56A,H56B,H56C),
 C57(H57A,H57B,H57C), C5(H5A,H5B,H5C), C9A(H9AA,H9AB,H9AC)
;
_shelx_res_checksum              6737
_olex2_submission_special_instructions 'No special instructions were received'