Modular Attachment of Appended Boron Lewis Acids to a Ruthenium Pincer Catalyst: Metal-Ligand Cooperativity Enables Selective Alkyne Hydrogenation.
Tseng, Kuei-Nin T; Kampf, Jeff W.; Szymczak, Nathaniel K.; Journal of the American Chemical Society 138 (2016) 10378–10381; doi:10.1021/jacs.6b03972

data_4130481
_publ_section_title
;
 Modular Attachment of Appended Boron Lewis Acids to a Ruthenium Pincer
 Catalyst: Metal-Ligand Cooperativity Enables Selective Alkyne
 Hydrogenation.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10378
_journal_page_last               10381
_journal_paper_doi               10.1021/jacs.6b03972
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C46 H43 B N5 P Ru, 0.5(C6 H6)'
_chemical_formula_sum            'C49 H46 B N5 P Ru'
_chemical_formula_weight         847.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90.690(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2340(13)
_cell_length_b                   12.0654(2)
_cell_length_c                   18.1135(13)
_cell_measurement_reflns_used    29435
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.30
_cell_measurement_theta_min      2.40
_cell_volume                     3984.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      85(2)
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Saturn944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            59745
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.358
_diffrn_reflns_theta_min         3.663
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    3.887
_exptl_absorpt_correction_T_max  0.706
_exptl_absorpt_correction_T_min  0.442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
 Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.910
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         7421
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0724P)^2^+2.3927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7375
_reflns_number_total             7421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b03972_si_001.cif
_cod_data_source_block           kt3289
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               4130481
_shelx_estimated_absorpt_t_min   0.541
_shelx_estimated_absorpt_t_max   0.721
_shelxl_version_number           2014/6
_shelx_res_checksum              16607
_shelx_hkl_checksum              20512