Scope and Mechanistic Analysis for Chemoselective Hydrogenolysis of Carbonyl Compounds Catalyzed by a Cationic Ruthenium Hydride Complex with a Tunable Phenol Ligand.
Kalutharage, Nishantha; Yi, Chae S.; Journal of the American Chemical Society 137 (2015) 11105–11114; doi:10.1021/jacs.5b06097

data_4124362
_publ_section_title
;
 Scope and Mechanistic Analysis for Chemoselective Hydrogenolysis of
 Carbonyl Compounds Catalyzed by a Cationic Ruthenium Hydride Complex with
 a Tunable Phenol Ligand.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11105
_journal_page_last               11114
_journal_paper_doi               10.1021/jacs.5b06097
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C54 H80 O7 P2 Ru2, 2(C2 H4 O), B F4'
_chemical_formula_sum            'C58 H88 B F4 O9 P2 Ru2'
_chemical_formula_weight         1280.17
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                96.5819(10)
_cell_angle_beta                 100.9333(10)
_cell_angle_gamma                111.4618(15)
_cell_formula_units_Z            2
_cell_length_a                   11.44999(18)
_cell_length_b                   11.75213(19)
_cell_length_c                   23.6747(2)
_cell_measurement_reflns_used    31030
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.5080
_cell_measurement_theta_min      4.1530
_cell_volume                     2851.36(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0564267000
_diffrn_orient_matrix_UB_12      0.0324382000
_diffrn_orient_matrix_UB_13      -0.0573661000
_diffrn_orient_matrix_UB_21      -0.1095043000
_diffrn_orient_matrix_UB_22      0.0128853000
_diffrn_orient_matrix_UB_23      0.0257237000
_diffrn_orient_matrix_UB_31      0.0844108000
_diffrn_orient_matrix_UB_32      0.1395003000
_diffrn_orient_matrix_UB_33      0.0250093000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22228
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.71
_diffrn_reflns_theta_min         3.88
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.387
_exptl_absorpt_correction_T_max  0.792
_exptl_absorpt_correction_T_min  0.473
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1334
_exptl_crystal_size_max          0.2265
_exptl_crystal_size_mid          0.1198
_exptl_crystal_size_min          0.0692
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         22228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0902P)^2^+1.6792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                20291
_reflns_number_total             22228
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b06097_si_005.cif
_cod_data_source_block           yi2x5
_cod_original_cell_volume        2851.36(7)
_cod_database_code               4124362
_chemical_oxdiff_formula         'C58 H88 B1 F4 O9 P2 Ru2'
_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(H1), C7(H7), C13(H13), C19(H19), C25(H25), C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
  C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B)
2.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C43(H43), C44(H44), C45(H45), C50(H50), C51(H51), C52(H52), C53(H53)
2.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C54(H54A,H54B,H54C)
;