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_4063427
_publ_contact_author_address
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       Hiroharu Suzuki
    Department of Applied Chemistry,
       Graduate School of Science and Engineering,
       Tokyo Institute of Technology,
       O-okayama, Meguro-ku, Tokyo
       152-8552, Japan 

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_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
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_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            'C47 H67 B Ir N3 O Ru'
_chemical_formula_weight         994.12
_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                94.572(18)
_cell_angle_beta                 107.210(12)
_cell_angle_gamma                89.502(14)
_cell_formula_units_Z            2
_cell_length_a                   13.6186(19)
_cell_length_b                   15.153(2)
_cell_length_c                   11.441(2)
_cell_measurement_temperature    243(2)
_cell_volume                     2247.8(6)
_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_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_measurement_method       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10753
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    3.330
_exptl_absorpt_correction_T_max  0.7319
_exptl_absorpt_correction_T_min  0.4349
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.418
_refine_diff_density_min         -4.077
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         10319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1045P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1371
_reflns_number_gt                8623
_reflns_number_total             10319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900692j_si_002.cif
_cod_data_source_block           complex3BPh4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4063427