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_4514291
_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         'C24 H22 Cl N2 Ru, Cl, 3.95(O)'
_chemical_formula_sum            'C24 H22 Cl2 N2 O3.95 Ru'
_chemical_formula_weight         573.6
_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             2017-10-26T14:28:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                92.790(6)
_cell_angle_beta                 99.326(4)
_cell_angle_gamma                96.309(4)
_cell_formula_units_Z            2
_cell_length_a                   6.9529(2)
_cell_length_b                   11.5712(7)
_cell_length_c                   16.8700(13)
_cell_measurement_reflns_used    2883
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      26.591
_cell_measurement_theta_min      2.437
_cell_measurement_wavelength     0.71073
_cell_volume                     1328.14(14)
_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 16.2439
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_details
;
  1 omega  -13.00   98.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767   38.0000   60.0000 111

  2 omega   83.00  118.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767 -178.0000    0.0000 35

  3 omega  -41.00   54.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  -77.0000  120.0000 95

  4 omega  -43.00   61.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  -38.0000  120.0000 104

  5 omega  -33.00   55.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  -57.0000 -120.0000 88

  6 omega   63.00  117.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  178.0000  150.0000 54

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0109619
_diffrn_orient_matrix_UB_12      0.047069
_diffrn_orient_matrix_UB_13      0.0267952
_diffrn_orient_matrix_UB_21      0.0516971
_diffrn_orient_matrix_UB_22      -0.0268148
_diffrn_orient_matrix_UB_23      0.0324898
_diffrn_orient_matrix_UB_31      0.0897197
_diffrn_orient_matrix_UB_32      0.0297742
_diffrn_orient_matrix_UB_33      -0.0070898
_diffrn_radiation_monochromator  'Multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_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            9376
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         28.315
_diffrn_reflns_theta_min         1.775
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.906
_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. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             579
_exptl_crystal_size_max          0.2264
_exptl_crystal_size_mid          0.0641
_exptl_crystal_size_min          0.0345
_refine_diff_density_max         1.555
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         9376
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0767
_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^)+(0.1317P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1942
_refine_ls_wR_factor_ref         0.2107
_reflns_number_gt                6419
_reflns_number_total             9376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b02958_si_004.cif
_cod_data_source_block           Zfreixa4
_cod_depositor_comments
'Adding full bibliography for 4514290--4514292.cif.'
_cod_original_cell_volume        1328.15(14)
_cod_database_code               4514291