Synthesis and Structure of a Novel Ruthenium Hydrido Bis(dihydrogen) Complex with 1,4,7-Trimethyl-1,4,7-triazacyclononane Ligand: A Useful Precursor for Synthesis of Heterometallic Complexes
Shima, Takanori; Namura, Kyo; Kameo, Hajime; Kakuta, Satoshi; Suzuki, Hiroharu; Organometallics 29 (2010) 337–; doi:10.1021/om900692j

data_4063429
_publ_contact_author_address
;
       Hiroharu Suzuki
    Department of Applied Chemistry,
       Graduate School of Science and Engineering,
       Tokyo Institute of Technology,
       O-okayama, Meguro-ku, Tokyo
       152-8552, Japan 

;
_publ_contact_author_email       hiroharu@o.cc.titech.ac.jp
_publ_contact_author_fax         '+81 3 5734 3913'
_publ_contact_author_phone       '+81 3 5734 2148'
_publ_section_title
;
 Synthesis and Structure of a Novel Ruthenium Hydrido Bis(dihydrogen)
 Complex with 1,4,7-Trimethyl-1,4,7-triazacyclononane Ligand: A Useful
 Precursor for Synthesis of Heterometallic Complexes
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              337
_journal_paper_doi               10.1021/om900692j
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C61 H73 B Ir N3 P Ru'
_chemical_formula_weight         1183.27
_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                114.322(4)
_cell_angle_beta                 92.068(2)
_cell_angle_gamma                99.0750(10)
_cell_formula_units_Z            2
_cell_length_a                   14.1656(10)
_cell_length_b                   14.5411(8)
_cell_length_c                   15.0940(8)
_cell_measurement_temperature    243(2)
_cell_volume                     2780.0(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'SHELXS-97 (Sheldrick, 1990)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      243(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku Rotating Anode Ultrax18'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18579
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    2.731
_exptl_absorpt_correction_T_max  0.6111
_exptl_absorpt_correction_T_min  0.3421
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1202
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         4.131
_refine_diff_density_min         -2.066
_refine_diff_density_rms         0.186
_refine_ls_extinction_coef       0.0090(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         11767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0882P)^2^+7.2222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                11056
_reflns_number_total             11767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900692j_si_002.cif
_cod_data_source_block           complex5BPh4
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4063429