Application of β-Diketiminato Arene-Substituted Ru(II) Complexes in Highly Efficient H2Dehydrocoupling of Amine Boranes
Schreiber, Dominique F.; O’Connor, Crystal; Grave, Christian; Ortin, Yannick; Müller-Bunz, Helge; Phillips, Andrew D.; ACS Catalysis 2 (2012) 2505–; doi:10.1021/cs300499d

data_4507138
_publ_section_title
;
 Application of \b-Diketiminato Arene-Substituted Ru(II) Complexes in
 Highly Efficient H2Dehydrocoupling of Amine Boranes
;
_journal_issue                   12
_journal_name_full               'ACS Catalysis'
_journal_page_first              2505
_journal_paper_doi               10.1021/cs300499d
_journal_volume                  2
_journal_year                    2012
_chemical_formula_moiety         'C31 H39 N2 Ru, C H Cl3, C1 F3 O3 S'
_chemical_formula_sum            'C33 H40 Cl3 F3 N2 O3 Ru S'
_chemical_formula_weight         809.15
_chemical_name_common            p-CymeneRu(2,6-Me2NacNac)OTf
_space_group_IT_number           2
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.72(2)
_cell_angle_beta                 71.49(3)
_cell_angle_gamma                64.83(2)
_cell_formula_units_Z            2
_cell_length_a                   10.788(2)
_cell_length_b                   12.131(5)
_cell_length_c                   16.206(5)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.872
_cell_measurement_theta_min      3.401
_cell_volume                     1799.1(11)
_computing_cell_refinement
'Dirax/lsq (Duisenberg A.J.M., Nonius B.V., 1989-2000)'
_computing_data_collection
'Collect (Hooft, R.W.W., 1998. Nonius B.V., 1997-2000)'
_computing_data_reduction        'EvalCCD (Hooft R.W.W., Nonius B.V., 1998)'
_computing_molecular_graphics
'Diamond 3.2 (Brandenburg, K., Crystal Impact GbR, 2009)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick G.M., Bruker AXS, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick G.M., Bruker AXS, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Apex II 95mm CCD camera'
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker-Nonus KappaCCD with \k-goniostat'
_diffrn_measurement_method       'squential \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonus (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_sigmaI/netI    0.0886
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23449
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.34
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Bruker Nonius Area Dector Scaling and Absorption Correction
SADABS 2.10 (Bruker, 2003)
based on an algorithm described by
R.H. Blessing, Acta Cryst. (1995), a51, 33-38
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.395
_exptl_crystal_size_mid          0.291
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.888
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         6213
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+11.4505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1386
_reflns_number_gt                4540
_reflns_number_total             6213
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cs300499d_si_001.cif
_cod_data_source_block           adp143
_cod_original_cell_volume        1799.2(10)
_cod_database_code               4507138