Identifying and Evading Olefin Isomerization Catalyst Deactivation Pathways Resulting from Ion-Tunable Hemilability
Dodge, Henry M.; Kita, Matthew R.; Chen, Chun-Hsing; Miller, Alexander J. M.; ACS Catalysis  (2020) 13019–13030; doi:10.1021/acscatal.0c03784

data_4518176
_publ_section_title
;
 Identifying and Evading Olefin Isomerization Catalyst Deactivation
 Pathways Resulting from Ion-Tunable Hemilability
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              13019
_journal_page_last               13030
_journal_paper_doi               10.1021/acscatal.0c03784
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C97 H72 B2 F48.00 Ir1.00 Li1.00 N1.00 O5.00 P1.00'
_chemical_formula_sum            'C97 H72 B2 F48 Ir Li N O5 P'
_chemical_formula_weight         2495.31
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2020-03-21
_audit_creation_method           CRYSTALS_ver_14.61_build_6236
_cell_angle_alpha                80.1550(10)
_cell_angle_beta                 89.5040(10)
_cell_angle_gamma                66.4130(10)
_cell_formula_units_Z            1
_cell_length_a                   12.8158(2)
_cell_length_b                   12.8715(2)
_cell_length_c                   17.2525(3)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    150
_cell_measurement_theta_max      69
_cell_measurement_theta_min      4
_cell_volume                     2564.14(8)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            54166
_diffrn_reflns_theta_full        25.606
_diffrn_reflns_theta_max         69.205
_diffrn_reflns_theta_min         3.772
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.929
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.37
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate fragment'
_exptl_crystal_F_000             1238
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.050
_refine_diff_density_max         4.03
_refine_diff_density_min         -0.86
_refine_ls_abs_structure_details 'Flack (1983), 6667 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.454(9)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1545
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1753
_refine_ls_number_reflns         16454
_refine_ls_number_restraints     878
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0865
_refine_ls_shift/su_max          0.0246485
_refine_ls_shift/su_mean         0.0022195
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.20P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2306
_refine_ls_wR_factor_gt          0.2298
_refine_ls_wR_factor_ref         0.2306
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              19
_reflns_limit_l_min              -20
_reflns_number_gt                16327
_reflns_number_total             16499
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.56
_oxford_diffrn_Wilson_scale      184.41
_oxford_refine_ls_r_factor_ref   0.0869
_oxford_refine_ls_scale          0.09401(7)
_oxford_reflns_number_all        16454
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '19028_0m_a.res in P1'
_cod_data_source_file            cs0c03784_si_003.cif
_cod_data_source_block           19028
_cod_original_sg_symbol_H-M      'P 1 '
_cod_original_formula_sum
'C97 H72 B2 F48.00 Ir1.00 Li1.00 N1.00 O5.00 P1.00'
_cod_database_code               4518176