Catalytic Dehydrogenation of Alkanes by PCP‒Pincer Iridium Complexes Using Proton and Electron Acceptors
Shada, Arun Dixith Reddy; Miller, Alexander J. M.; Emge, Thomas J.; Goldman, Alan S.; ACS Catalysis  (2021) 3009–3016; doi:10.1021/acscatal.0c05160

data_4518501
_publ_section_title
;
 Catalytic Dehydrogenation of Alkanes by PCP--Pincer Iridium Complexes
 Using Proton and Electron Acceptors
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              3009
_journal_page_last               3016
_journal_paper_doi               10.1021/acscatal.0c05160
_journal_year                    2021
_chemical_formula_moiety
; 
(C24 H41 O P2 Ir)+,(B F4)- 
;
_chemical_formula_sum            'C24 H46 B F4 Ir O P2'
_chemical_formula_weight         691.56
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.1482(14)
_cell_length_b                   16.0706(13)
_cell_length_c                   21.2524(17)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.26
_cell_measurement_theta_min      2.38
_cell_volume                     5856.8(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  SHELXL-2014/7
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            69464
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.246
_diffrn_reflns_theta_min         1.916
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    4.708
_exptl_absorpt_correction_T_max  0.63656
_exptl_absorpt_correction_T_min  0.24100
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SAINT (SADABS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.702
_refine_diff_density_min         -1.481
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         9453
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0296P)^2^+9.8509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7562
_reflns_number_total             9453
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c05160_si_002.cif
_cod_data_source_block           arun_PCPIrH_aquo_BF4_Pbca
_cod_database_code               4518501
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.332
_shelx_estimated_absorpt_t_max   0.704
_exptl_absorpt_special_details
; 
(C24 H41 O P2 Ir)+,(B F4)- 
;
_shelx_res_checksum              91636
_shelx_hkl_checksum              4154