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_4063426
_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            'C9 H26 F6 N3 P Ru'
_chemical_formula_weight         422.37
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.0460(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6272(4)
_cell_length_b                   9.7739(3)
_cell_length_c                   14.2836(6)
_cell_measurement_reflns_used    18743
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      3.55
_cell_volume                     1570.06(10)
_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      153(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0152
_diffrn_reflns_av_sigmaI/netI    0.0126
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18743
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    1.156
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7999
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.0008(3)
_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   1.105
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         4564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0346P)^2^+1.2465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0697
_reflns_number_gt                4094
_reflns_number_total             4833
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900692j_si_002.cif
_cod_data_source_block           complex2PF6
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' 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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4063426