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_4514290
_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         'C20 H20 Cl N8 Ru, Cl'
_chemical_formula_sum            'C20 H20 Cl2 N8 Ru'
_chemical_formula_weight         544.41
_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             2016-05-24T16:47:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                98.121(6)
_cell_angle_beta                 99.958(7)
_cell_angle_gamma                116.027(7)
_cell_formula_units_Z            2
_cell_length_a                   9.4232(7)
_cell_length_b                   10.4405(5)
_cell_length_c                   14.3166(12)
_cell_measurement_reflns_used    3338
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.288
_cell_measurement_theta_min      3.205
_cell_measurement_wavelength     1.54184
_cell_volume                     1208.50(18)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2012
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
  1 omega -101.00    4.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.5756  -19.0000   30.0000 105

  2 omega -107.00  -25.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.5756  -38.0000  -30.0000 82

  3 omega   40.00  121.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       39.5756 -178.0000  -60.0000 81

  4 omega  -41.00  -10.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000   61.0000   90.0000 31

  5 omega  -40.00  -13.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000   30.0000 -150.0000 27

  6 omega -121.00  -14.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  125.0000 -120.0000 107

  7 omega   33.00   60.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -30.0000  150.0000 27

  8 omega   61.00  121.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109 -125.0000  -60.0000 60

  9 omega   32.00  143.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -77.0000   90.0000 111

 10 omega   42.00  121.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109 -125.0000   90.0000 79

 11 omega   86.00  130.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109   45.0000 -180.0000 44

 12 omega   32.00   68.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -30.0000 -120.0000 36

 13 omega   37.00   64.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -30.0000  -90.0000 27

 14 omega   52.00  143.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -77.0000  -90.0000 91

 15 omega   38.00   65.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -30.0000    0.0000 27

 16 omega   35.00   66.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -30.0000 -150.0000 31

 17 omega   30.00   58.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -94.0000  150.0000 28

 18 omega   83.00  108.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -94.0000  150.0000 25

 19 omega   58.00  157.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109   15.0000  150.0000 99

 20 omega   32.00   67.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109  -30.0000 -180.0000 35

 21 omega   79.00  157.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6109   30.0000   30.0000 78
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0355105
_diffrn_orient_matrix_UB_12      -0.1408447
_diffrn_orient_matrix_UB_13      0.0356164
_diffrn_orient_matrix_UB_21      -0.0782809
_diffrn_orient_matrix_UB_22      -0.0924543
_diffrn_orient_matrix_UB_23      -0.1065653
_diffrn_orient_matrix_UB_31      0.1679095
_diffrn_orient_matrix_UB_32      0.0175135
_diffrn_orient_matrix_UB_33      -0.0087162
_diffrn_radiation_monochromator  'Multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7871
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.994
_diffrn_reflns_theta_min         3.233
_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    7.419
_exptl_absorpt_correction_T_max  0.778
_exptl_absorpt_correction_T_min  0.548
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.1431
_exptl_crystal_size_mid          0.0561
_exptl_crystal_size_min          0.0399
_refine_diff_density_max         2.462
_refine_diff_density_min         -1.486
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4398
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0799
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1043P)^2^+15.1642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2203
_refine_ls_wR_factor_ref         0.2324
_reflns_number_gt                3717
_reflns_number_total             4398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b02958_si_001.cif
_cod_data_source_block           Zfreixa_8
_cod_depositor_comments
'Adding full bibliography for 4514290--4514292.cif.'
_cod_original_cell_volume        1208.50(15)
_cod_database_code               4514290