Synthesis and N-H Reductive Elimination Study of Dinuclear Ruthenium Imido Dihydride Complexes
Shin Takemoto; Yusuke Yamazaki; Takahiro Yamano; Daichi Mashima; Hiroyuki Matsuzaka; Journal of the American Chemical Society 134 (2012) 17027–17035; doi:10.1021/ja3005682

data_4118750
_publ_section_title
;
 Synthesis and N-H Reductive Elimination Study of Dinuclear Ruthenium
 Imido Dihydride Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17027
_journal_page_last               17035
_journal_paper_doi               10.1021/ja3005682
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C36 H45 N Ru2'
_chemical_formula_weight         693.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                105.741(12)
_cell_angle_beta                 94.616(12)
_cell_angle_gamma                90.083(15)
_cell_formula_units_Z            4
_cell_length_a                   12.088(4)
_cell_length_b                   15.545(6)
_cell_length_c                   17.205(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3100.7(18)
_computing_cell_refinement       'rigaku process auto'
_computing_data_collection       'rigaku process auto'
_computing_data_reduction        'rigaku process auto'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'rigaku r-axis rapid'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29938
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.999
_exptl_absorpt_correction_T_max  0.9803
_exptl_absorpt_correction_T_min  0.6908
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   abscor
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       plate
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         13974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.9309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1137
_reflns_number_gt                10046
_reflns_number_total             13974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3005682_si_001_2.cif
_cod_data_source_block           5a
_cod_original_cell_volume        3100.9(18)
_cod_database_code               4118750