Hydride-Bridged NiRh Complexes with Tunable N3S2Dithiolato Ligands and Their Utilization as Catalysts for Hydrogenation of Aldehydes and CO2in Aqueous Media
Kure, Bunsho; Taniguchi, Ayami; Nakajima, Takayuki; Tanase, Tomoaki; Organometallics 31 (2012) 4791–; doi:10.1021/om300350u

data_4078707
_publ_section_title
;
 Hydride-Bridged NiRh Complexes with Tunable N3S2Dithiolato Ligands and
 Their Utilization as Catalysts for Hydrogenation of Aldehydes and CO2in
 Aqueous Media
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              4791
_journal_paper_doi               10.1021/om300350u
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C13 H27 N3 Ni S2'
_chemical_formula_sum            'C13 H27 N3 Ni S2'
_chemical_formula_weight         348.20
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.418(14)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.163(15)
_cell_length_b                   17.29(4)
_cell_length_c                   12.29(3)
_cell_measurement_reflns_used    2123
_cell_measurement_temperature    153
_cell_measurement_theta_max      27.09
_cell_measurement_theta_min      3.19
_cell_volume                     1734(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      153
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7293
_diffrn_reflns_theta_full        26.87
_diffrn_reflns_theta_max         26.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.352
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             744.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.510
_refine_diff_density_min         -0.820
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1625 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.91(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3474
_refine_ls_number_restraints     2
_refine_ls_R_factor_gt           0.0770
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1222P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2237
_reflns_number_gt                2087
_reflns_number_total             3474
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om300350u_si_002.cif
_cod_data_source_block           complex1b
_cod_original_cell_volume        1734(6)
_cod_database_code               4078707