Rigid Postmetallocene Catalysts for Propylene Polymerization: Ligand Design Prevents the Temperature-Dependent Loss of Stereo- and Regioselectivities
Goryunov, Georgy P.; Sharikov, Mikhail I.; Iashin, Andrei N.; Canich, Jo Ann M.; Mattler, Sarah J.; Hagadorn, John R.; Uborsky, Dmitry V.; Voskoboynikov, Alexander Z.; ACS Catalysis 11 (2021) 8079–8086; doi:10.1021/acscatal.1c01611

data_4518828
_publ_section_title
;
 Rigid Postmetallocene Catalysts for Propylene Polymerization: Ligand
 Design Prevents the Temperature-Dependent Loss of Stereo- and
 Regioselectivities
;
_journal_issue                   13
_journal_name_full               'ACS Catalysis'
_journal_page_first              8079
_journal_page_last               8086
_journal_paper_doi               10.1021/acscatal.1c01611
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C55 H61 Hf N O2'
_chemical_formula_sum            'C55 H61 Hf N O2'
_chemical_formula_weight         946.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.4480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.0406(16)
_cell_length_b                   16.9643(9)
_cell_length_c                   19.5677(11)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.57
_cell_measurement_theta_min      2.30
_cell_volume                     9413.5(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            56610
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.997
_diffrn_reflns_theta_min         1.436
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.257
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.3489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0884 before and 0.0412 after correction. The Ratio of minimum to maximum transmission is 0.8150. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       prism
_exptl_crystal_F_000             3888
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.281
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         12484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+17.1659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0517
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10986
_reflns_number_total             12484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c01611_si_002.cif
_cod_data_source_block           sad
_cod_depositor_comments          'Adding full bibliography for 4518828.cif.'
_cod_database_code               4518828
_shelxl_version_number           2014/6
_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. Uiso/Uaniso restraints and constraints
Uanis(O1) = Uanis(O2)
3.a Ternary CH refined with riding coordinates:
 C15(H15), C17(H17), C19(H19), C42(H42), C44(H44), C46(H46)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C16(H16A,H16B), C18(H18A,H18B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C41(H41A,H41B), C43(H43A,H43B), C45(H45A,H45B),
 C47(H47A,H47B), C48(H48A,H48B), C55(H55A,H55B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C9(H9), C11(H11), C24(H24), C25(H25), C26(H26),
 C30(H30), C31(H31), C33(H33), C36(H36), C38(H38)
3.d Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              93908
_shelx_hkl_checksum              71159
_shelx_fab_checksum              1517
_olex2_submission_special_instructions 'No special instructions were received'