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_4518515
_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         'C33 H63 N2 Si2 Ti2, C H B11 Cl11, C6 H5 F'
_chemical_formula_sum            'C40 H69 B11 Cl11 F N2 Si2 Ti2'
_chemical_formula_weight         1257.81
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                83.8800(10)
_cell_angle_beta                 75.3620(10)
_cell_angle_gamma                85.7830(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1095(13)
_cell_length_b                   15.0642(17)
_cell_length_c                   17.4165(19)
_cell_measurement_reflns_used    9848
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      27.471
_cell_measurement_theta_min      4.745
_cell_volume                     3052.9(6)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0483
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            70947
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         4.542
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0633 before and 0.0522 after correction. The Ratio of minimum to maximum transmission is 0.8404. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       plate
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.638
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.134
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         10651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+3.7505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8579
_reflns_number_total             10651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c04228_si_002.cif
_cod_data_source_block           sogwca156
_cod_depositor_comments
'Adding full bibliography for 4518514--4518515.cif.'
_cod_database_code               4518515
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.624
_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.a Riding coordinates:
 C17(H17A,H17B,H17C)
2.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C37(H37), C38(H38), C39(H39), C40(H40)
2.c 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), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C)
2.d Boron cage BH refined with riding coordinates:
 C34(H34)
;
_shelx_res_checksum              93388
_shelx_hkl_checksum              42255
_olex2_submission_special_instructions 'No special instructions were received'