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_4514698
_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_sum            'C38 H62 P2 Ru S'
_chemical_formula_weight         713.94
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 105.1762(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2907(13)
_cell_length_b                   15.6689(14)
_cell_length_c                   18.8836(18)
_cell_measurement_reflns_used    9064
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.48
_cell_measurement_theta_min      2.38
_cell_volume                     3795.4(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.0830
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37978
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         1.714
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker (SAINT)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       plate
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.551
_refine_diff_density_min         -1.326
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         10200
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+7.4969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7699
_reflns_number_total             10200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b05172_si_004.cif
_cod_data_source_block           RuPSPprop_P21c
_cod_database_code               4514698
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.833
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              44789
_shelx_hkl_checksum              13041