Experimental Evidence Supporting Related Mechanisms for Ru(II)-Catalyzed Dehydrocoupling and Hydrolysis of Amine-Boranes
Telleria, Ainara; Vicent, Cristian; San Nacianceno, Virginia; Garralda, María A.; Freixa, Zoraida; ACS Catalysis 7 (2017) 8394–; doi:10.1021/acscatal.7b02958

data_4514292
_publ_section_title
;
 Experimental Evidence Supporting Related Mechanisms for Ru(II)-Catalyzed
 Dehydrocoupling and Hydrolysis of Amine-Boranes
;
_journal_issue                   12
_journal_name_full               'ACS Catalysis'
_journal_page_first              8394
_journal_paper_doi               10.1021/acscatal.7b02958
_journal_volume                  7
_journal_year                    2017
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C23 H23 Br1 Cl11 N5 Ru1'
_chemical_formula_sum            'C23 H23 Br Cl11 N5 Ru'
_chemical_formula_weight         940.39
_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_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_audit_creation_date             2016-05-24T15:44:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                93.576(7)
_cell_angle_beta                 102.190(7)
_cell_angle_gamma                107.715(7)
_cell_formula_units_Z            2
_cell_length_a                   10.6051(8)
_cell_length_b                   10.7857(9)
_cell_length_c                   16.5095(15)
_cell_measurement_reflns_used    4310
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.5567
_cell_measurement_theta_min      2.7616
_cell_measurement_wavelength     1.54184
_cell_volume                     1742.0(3)
_computing_cell_refinement
'CrysAlis Pro (Oxford Diffraction Ltd., 2011)'
_computing_data_collection
'CrysAlis Pro (Oxford Diffraction Ltd., 2011)'
_computing_data_reduction
'CrysAlis Pro (Oxford Diffraction Ltd., 2011)'
_computing_molecular_graphics    'Diamond v.3.2f (Crystal Impact GbR, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'OLEX2 (Dolomanov et al, 2009)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4023
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -49.00   49.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5756    0.0000  150.0000 98

  2 omega -116.00  -15.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5756  -38.0000  -30.0000 101

  3 omega    6.00   52.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5756 -125.0000 -120.0000 46

  4 omega   28.00   86.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5756 -125.0000  150.0000 58

  5 omega   30.00   90.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5756 -125.0000  -30.0000 60

  6 omega   35.00   62.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000  -90.0000 27

  7 omega   42.00   69.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000   60.0000 27

  8 omega   92.00  122.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -77.0000  -90.0000 30

  9 omega   32.00   57.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000 -150.0000 25

 10 omega   30.00   59.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000  -60.0000 29

 11 omega   28.00   54.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609 -104.0000  -47.0000 26

 12 omega   33.00   64.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609 -125.0000   90.0000 31

 13 omega   73.00  119.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609 -125.0000   90.0000 46

 14 omega   31.00  133.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -77.0000 -180.0000 102

 15 omega   37.00   77.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000 -180.0000 40

 16 omega   92.00  157.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   61.0000   90.0000 65

 17 omega   88.00  121.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609 -125.0000 -120.0000 33

 18 omega   36.00   75.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000  -30.0000 39

 19 omega   38.00   75.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000  -90.0000 37

 20 omega   43.00  103.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -61.0000   30.0000 60

 21 omega  104.00  132.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -61.0000   30.0000 28

 22 omega  129.00  154.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   45.0000 -120.0000 25

 23 omega   26.00  144.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -15.0000   90.0000 118

 24 omega   70.00  103.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609 -104.0000  -47.0000 33

 25 omega   65.00  103.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000  120.0000 38
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0573865
_diffrn_orient_matrix_UB_12      0.0090399
_diffrn_orient_matrix_UB_13      -0.092481
_diffrn_orient_matrix_UB_21      -0.1418696
_diffrn_orient_matrix_UB_22      -0.0890312
_diffrn_orient_matrix_UB_23      0.0048447
_diffrn_orient_matrix_UB_31      -0.0358132
_diffrn_orient_matrix_UB_32      0.1220589
_diffrn_orient_matrix_UB_33      0.0266321
_diffrn_radiation_monochromator  'Multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Nova (Cu) X-ray micro-source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.1311
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12176
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.99
_diffrn_reflns_theta_min         2.764
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    12.961
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.68944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.793
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.629
_refine_diff_density_min         -1.492
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         6553
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1108P)^2^+1.8784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1847
_reflns_number_gt                5386
_reflns_number_total             6553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b02958_si_002.cif
_cod_data_source_block           Zfreixa_10
_cod_depositor_comments
'Adding full bibliography for 4514290--4514292.cif.'
_cod_database_code               4514292