Controlled Ring-Opening Polymerization of β-Butyrolactone Via Bifunctional Organoboron Catalysts
Yang, Li; Zhang, Yao-Yao; Yang, Guan-Wen; Xie, Rui; Wu, Guang-Peng; Macromolecules  (2021) –; doi:10.1021/acs.macromol.1c00250

data_1562940
_publ_section_title
;
 Controlled Ring-Opening Polymerization of \b-Butyrolactone Via
 Bifunctional Organoboron Catalysts
;
_journal_name_full               Macromolecules
_journal_paper_doi               10.1021/acs.macromol.1c00250
_journal_year                    2021
_chemical_formula_moiety         'C24 H40 B N O2'
_chemical_formula_sum            'C24 H40 B N O2'
_chemical_formula_weight         385.38
_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             2021-02-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.386(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8723(11)
_cell_length_b                   9.8390(9)
_cell_length_c                   16.6022(12)
_cell_measurement_reflns_used    6193
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      27.113
_cell_measurement_theta_min      2.365
_cell_volume                     2229.8(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16436
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.192
_diffrn_reflns_theta_min         2.365
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1602 before and 0.0572 after correction. The Ratio of minimum to maximum transmission is 0.8554. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       needle
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4925
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0640
_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^)+(0.0795P)^2^+1.5446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1773
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3881
_reflns_number_total             4925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma1c00250_si_002.cif
_cod_data_source_block           1e
_cod_database_code               1562940
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.980
_olex2_refinement_description
;
1. Restrained distances
 C5-C4
 1.45 with sigma of 0.01
 C4-C5
 1.45 with sigma of 0.01
 C5-C6
 1.45 with sigma of 0.001
 C5A-C4
 1.45 with sigma of 0.01
2. Others
 Fixed Sof: H4bc(0.75) H4bd(0.75) H4aa(0.25) H4ab(0.25) C5(0.6) H5a(0.6)
 H5b(0.6) C6(0.6) H6a(0.6) H6c(0.6) H6b(0.6) C5A(0.4) H5Aa(0.4) H5Ab(0.4)
 C6A(0.4) H6Aa(0.4) H6Ac(0.4) H6Ab(0.4)
;
_shelx_res_checksum              56595
_shelx_hkl_checksum              52380
_olex2_submission_special_instructions 'No special instructions were received'