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_4130480
_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         'C50 H52 B2 N5 O4 P Ru, 1.5(C6 H6)'
_chemical_formula_sum            'C59 H61 B2 N5 O4 P Ru'
_chemical_formula_weight         1057.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.8335(3)
_cell_length_b                   12.51430(10)
_cell_length_c                   39.2291(6)
_cell_measurement_reflns_used    34558
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.9710
_cell_measurement_theta_min      2.2630
_cell_volume                     10227.7(2)
_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_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1317
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            155905
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.424
_diffrn_reflns_theta_min         2.121
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    3.198
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27523
_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            black
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       plate
_exptl_crystal_F_000             4408
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.406
_refine_diff_density_min         -1.193
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details
; 
 Flack x determined using 6820 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.002(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1316
_refine_ls_number_reflns         17961
_refine_ls_number_restraints     343
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0697
_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^)+(0.0740P)^2^+83.6222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1875
_refine_ls_wR_factor_ref         0.1906
_reflns_Friedel_coverage         0.968
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                16576
_reflns_number_total             17961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b03972_si_001.cif
_cod_data_source_block           kt3236
_cod_depositor_comments
;

2020-05-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C50 H52 B2 N5 O4 P Ru), 3(C6 H6)'
_cod_original_formula_sum        'C118 H122 B4 N10 O8 P2 Ru2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     2115.57
_cod_database_code               4130480
_shelxl_version_number           2014/6
_shelx_res_checksum              14649
_shelx_hkl_checksum              81618