Tris(2,4-difluorophenyl)borane/Triisobutylphosphine Lewis Pair: A Thermostable and Air/Moisture-Tolerant Organic Catalyst for the Living Polymerization of Acrylates
Zhang, Zhen-Hua; Wang, Xing; Wang, Xiao-Jun; Li, Yuesheng; Hong, Miao; Macromolecules 54 (2021) 8495–8502; doi:10.1021/acs.macromol.1c01356

data_1564812
_publ_section_title
;
 Tris(2,4-difluorophenyl)borane/Triisobutylphosphine Lewis Pair: A
 Thermostable and Air/Moisture-Tolerant Organic Catalyst for the Living
 Polymerization of Acrylates
;
_journal_issue                   18
_journal_name_full               Macromolecules
_journal_page_first              8495
_journal_page_last               8502
_journal_paper_doi               10.1021/acs.macromol.1c01356
_journal_volume                  54
_journal_year                    2021
_chemical_formula_moiety         'C30 H36 B F6 P'
_chemical_formula_sum            'C30 H36 B F6 P'
_chemical_formula_weight         552.37
_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             2020-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.579(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6365(9)
_cell_length_b                   19.960(2)
_cell_length_c                   16.4399(17)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      55.02
_cell_measurement_theta_min      5.09
_cell_volume                     2815.3(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      169.99
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30418
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.036
_diffrn_reflns_theta_min         3.042
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.883
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1368 before and 0.0709 after correction. The Ratio of minimum to maximum transmission is 0.7468. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+1.1772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.0970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5133
_reflns_number_total             5342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma1c01356_si_001.cif
_cod_data_source_block           mj20282_0m
_cod_original_cell_volume        2815.4(5)
_cod_database_code               1564812
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.933
_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.a Ternary CH refined with riding coordinates:
 C20(H20), C24(H24), C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C23(H23A,H23B), C27(H27A,H27B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C9(H9), C11(H11), C12(H12), C15(H15), C17(H17),
 C18(H18)
2.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              20772
_shelx_hkl_checksum              80789
_olex2_submission_special_instructions 'No special instructions were received'