Highly Efficient Carborane-Based Activators for Molecular Olefin Polymerization Catalysts
Gunther, S. Olivia; Lai, Qingheng; Senecal, Todd; Huacuja, Rafael; Bremer, Sean; Pearson, David M.; DeMott, Jessica C.; Bhuvanesh, Nattamai; Ozerov, Oleg V.; Klosin, Jerzy; ACS Catalysis 11 (2021) 3335–3342; doi:10.1021/acscatal.0c04228

data_4518514
_publ_section_title
;
 Highly Efficient Carborane-Based Activators for Molecular Olefin
 Polymerization Catalysts
;
_journal_issue                   6
_journal_name_full               'ACS Catalysis'
_journal_page_first              3335
_journal_page_last               3342
_journal_paper_doi               10.1021/acscatal.0c04228
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C19 H39 N2 Si Ti, C6 H5 F, C1 H1 B11 Cl11'
_chemical_formula_sum            'C26 H45 B11 Cl11 F N2 Si Ti'
_chemical_formula_weight         989.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.304(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.657(2)
_cell_length_b                   32.375(6)
_cell_length_c                   12.033(2)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      27.468
_cell_measurement_theta_min      2.517
_cell_volume                     4504.3(14)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2016)'
_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      110.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0399
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            106732
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.516
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.899
_exptl_absorpt_correction_T_max  0.4915
_exptl_absorpt_correction_T_min  0.3501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1019 before and 0.0514 after correction. The Ratio of minimum to maximum transmission is 0.7123. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.576
_exptl_crystal_size_mid          0.474
_exptl_crystal_size_min          0.228
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         7922
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0084P)^2^+10.5692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0983
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6912
_reflns_number_total             7922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c04228_si_003.cif
_cod_data_source_block           sogwca178
_cod_depositor_comments
'Adding full bibliography for 4518514--4518515.cif.'
_cod_original_cell_volume        4504.4(15)
_cod_database_code               4518514
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.626
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(B3) = Uanis(B3A)
Uanis(B2) = Uanis(B2A)
Uanis(B1) = Uanis(B1A)
Uanis(B4) = Uanis(B4A)
Uanis(B5) = Uanis(B5A)
Uanis(B6) = Uanis(B6A)
Uanis(B7) = Uanis(B7A)
Uanis(B8) = Uanis(B8A)
Uanis(B9) = Uanis(B9A)
Uanis(B10) = Uanis(B10A)
Uanis(B11) = Uanis(B11A)
Uanis(C20A) = Uanis(C20)
3. Same fragment restrains
{Cl10, Cl1, Cl2, Cl3, Cl4, Cl5, Cl6, Cl7, Cl8, Cl9, Cl11, C20, B1, B2, B3, B4,
B5, B6, B7, B8, B9, B10, B11} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl, Cl1A, Cl2A, Cl3A, Cl4A, Cl5A, Cl6A, Cl7A, Cl8A, Cl9A, Cl12, C20A, B1A,
B2A, B3A, B4A, B5A, B6A, B7A, B8A, B9A, B10A, B11A}
4. Others
 Sof(H1S)=Sof(F1S)=Sof(Cl)=Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=Sof(Cl4A)=Sof(Cl5A)=
 Sof(Cl6A)=Sof(Cl7A)=Sof(Cl8A)=Sof(Cl9A)=Sof(Cl12)=Sof(C20A)=Sof(H20A)=Sof(B1A)=
 Sof(B2A)=Sof(B3A)=Sof(B4A)=Sof(B5A)=Sof(B6A)=Sof(B7A)=Sof(B8A)=Sof(B9A)=
 Sof(B10A)=Sof(B11A)=1-FVAR(1)
 Sof(H3S)=Sof(F2S)=Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=Sof(Cl4)=Sof(Cl5)=Sof(Cl6)=
 Sof(Cl7)=Sof(Cl8)=Sof(Cl9)=Sof(Cl10)=Sof(Cl11)=Sof(C20)=Sof(H20)=Sof(B1)=
 Sof(B2)=Sof(B3)=Sof(B4)=Sof(B5)=Sof(B6)=Sof(B7)=Sof(B8)=Sof(B9)=Sof(B10)=
 Sof(B11)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C1S(H1S), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S)
5.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C)
5.c Boron cage BH refined with riding coordinates:
 C20(H20), C20A(H20A)
;
_shelx_res_checksum              78362
_shelx_hkl_checksum              30902
_olex2_submission_special_instructions 'No special instructions were received'