Deeper Mechanistic Insight into Ru Pincer-Mediated Acceptorless Dehydrogenative Coupling of Alcohols: Exchanges, Intermediates, and Deactivation Species
Nguyen, Duc Hanh; Trivelli, Xavier; Capet, Frédéric; Swesi, Youssef; Favre-Réguillon, Alain; Vanoye, Laurent; Dumeignil, Franck; Gauvin, Régis M.; ACS Catalysis 8 (2018) 4719–; doi:10.1021/acscatal.8b00995

data_4515579
_publ_section_title
;
 Deeper Mechanistic Insight into Ru Pincer-Mediated Acceptorless
 Dehydrogenative Coupling of Alcohols: Exchanges, Intermediates, and
 Deactivation Species
;
_journal_issue                   5
_journal_name_full               'ACS Catalysis'
_journal_page_first              4719
_journal_paper_doi               10.1021/acscatal.8b00995
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C19 H41 N O3 P2 Ru'
_chemical_formula_sum            'C19 H41 N O3 P2 Ru'
_chemical_formula_weight         494.54
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.1700(5)
_cell_length_b                   15.3918(6)
_cell_length_c                   21.7410(8)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.39
_cell_measurement_theta_min      2.17
_cell_volume                     4741.8(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0422
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            81145
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.453
_diffrn_reflns_theta_min         1.873
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.813
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0797 before and 0.0492 after correction.
The Ratio of minimum to maximum transmission is 0.9290.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       prism
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         7191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+2.2661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6139
_reflns_number_total             7191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b00995_si_003.cif
_cod_data_source_block           mo_dhng157
_cod_database_code               4515579
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1A), C11(H11), C14(H14), C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C7(H7A,H7B), C10(H10A,H10B), C8(H8A,H8B)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C15(H15A,H15B,H15C), C5(H5A,H5B,H5C), C16(H16A,H16B,
 H16C), C12(H12A,H12B,H12C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C13(H13A,H13B,
 H13C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              20687
_shelx_hkl_checksum              88219
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'