Catalytic Alkane Transfer Dehydrogenation by PSP-Pincer-Ligated Ruthenium. Deactivation of an Extremely Reactive Fragment by Formation of Allyl Hydride Complexes
Zhou, Xiaoguang; Malakar, Santanu; Zhou, Tian; Murugesan, Sathiyamoorthy; Huang, Carlos; Emge, Thomas J.; Krogh-Jespersen, Karsten; Goldman, Alan S.; ACS Catalysis 9 (2019) 4072–; doi:10.1021/acscatal.8b05172

data_4514697
_publ_section_title
;
 Catalytic Alkane Transfer Dehydrogenation by PSP-Pincer-Ligated
 Ruthenium. Deactivation of an Extremely Reactive Fragment by Formation of
 Allyl Hydride Complexes
;
_journal_issue                   5
_journal_name_full               'ACS Catalysis'
_journal_page_first              4072
_journal_paper_doi               10.1021/acscatal.8b05172
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety
; 
C39 H64 P2 Ru S, 0.5(C5 H12), 0.25(C6 H14)' 
;
_chemical_formula_sum            'C43 H73.5 P2 Ru S'
_chemical_formula_weight         785.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90.092(4)
_cell_angle_beta                 92.283(4)
_cell_angle_gamma                101.727(4)
_cell_formula_units_Z            4
_cell_length_a                   13.159(2)
_cell_length_b                   15.396(3)
_cell_length_c                   21.596(4)
_cell_measurement_reflns_used    4496
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.73
_cell_measurement_theta_min      2.28
_cell_volume                     4280.3(13)
_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 0.999
_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  0.0725
_diffrn_reflns_av_unetI/netI     0.1026
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            43045
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.582
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SAINT (SADABS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       rod
_exptl_crystal_F_000             1686
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.885
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         18868
_refine_ls_number_restraints     1099
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0660
_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^)+(0.0771P)^2^+2.0436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13062
_reflns_number_total             18868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b05172_si_003.cif
_cod_data_source_block           rupspeth2_P-1
_cod_original_cell_volume        4280.5(13)
_cod_original_formula_sum        'C43 H73.50 P2 Ru S'
_cod_database_code               4514697
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.873
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              17730
_shelx_hkl_checksum              31416