Pyridine-amido aluminum catalyst precursors for 1,3-butadiene transition-metal-free stereospecific polymerization
Tang, Jian; Xu, Zijian; Liu, Zelong; Fu, Yuan; Hua, Jing; Polymer Chemistry 14 (2023) 980–989; doi:10.1039/D2PY01093C

data_1568473
_publ_section_title
;
 Pyridine-amido aluminum catalyst precursors for 1,3-butadiene
 transition-metal-free stereospecific polymerization
;
_journal_issue                   8
_journal_name_full               'Polymer Chemistry'
_journal_page_first              980
_journal_page_last               989
_journal_paper_doi               10.1039/D2PY01093C
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C18 H19 Al F6 N2'
_chemical_formula_sum            'C18 H19 Al F6 N2'
_chemical_formula_weight         404.33
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-31
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-05-26 deposited with the CCDC.	2023-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                87.3090(10)
_cell_angle_beta                 77.9280(10)
_cell_angle_gamma                89.4530(10)
_cell_formula_units_Z            2
_cell_length_a                   8.5573(6)
_cell_length_b                   8.8128(6)
_cell_length_c                   13.3517(9)
_cell_measurement_reflns_used    4201
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      25.796
_cell_measurement_theta_min      2.313
_cell_volume                     983.55(12)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker SMART APEX II diffractrometer'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298.15
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11894
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.725
_diffrn_reflns_theta_min         1.561
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.162
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0710 before and 0.0429 after correction.
The Ratio of minimum to maximum transmission is 0.7200.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       block
_exptl_crystal_F_000             416
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-pentane'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4690
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0677P)^2^+0.1359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1431
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3166
_reflns_number_total             4690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2py01093c2.cif
_cod_data_source_block           211209e
_cod_depositor_comments
'Adding full bibliography for 1568468--1568473.cif.'
_cod_database_code               1568473
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.979
_exptl_crystal_mounting_method
'The title complex was mounted in a sealed capillary.'
_olex2_refinement_description
;
1. Restrained distances
 F2-C15 \\sim F1A-C15 \\sim F1-C15 \\sim F3A-C15 \\sim F3-C15 \\sim F2A-C15
 with sigma of 0.02
 F5A-C16 \\sim F5-C16 \\sim F6A-C16 \\sim F6-C16 \\sim F4A-C16 \\sim F4-C16
 with sigma of 0.02
 F5A-F4A \\sim F6A-F5A \\sim F6A-F4A
 with sigma of 0.02
 F6-F4 \\sim F5-F4 \\sim F6-F5
 with sigma of 0.02
 F3-F2 \\sim F2-F1 \\sim F3-F1
 with sigma of 0.02
 F3A-F2A \\sim F2A-F1A \\sim F3A-F1A
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
F5 \\sim F6 \\sim F6A \\sim F4 \\sim F5A \\sim F4A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
F1 \\sim F2 \\sim F3 \\sim F3A \\sim F2A \\sim F1A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
3. Rigid body (RIGU) restrains
 F2, C15, F1, F3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C16, F5, F4, F6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 F3A, C15, F2A, F1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C16, F5A, F4A, F6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Others
 Sof(F3A)=Sof(F1A)=Sof(F2A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F5A)=Sof(F6A)=Sof(F4A)=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C10(H10), C12(H12), C14(H14)
5.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              5788
_olex2_submission_special_instructions 'No special instructions were received'