Synthesis and Reactivities of Sulfido-bridged Ir‒W and Ir‒Re Heterodinuclear Complexes with Imido Ligands
Arashiba, Kazuya; Tanabe, Yoshiaki; Ishii, Youichi; Chemistry Letters 36 (2007) 622–; doi:10.1246/cl.2007.622

data_8000167
_publ_section_title
;
 Synthesis and Reactivities of Sulfido-bridged Ir--W and Ir--Re
 Heterodinuclear Complexes with Imido Ligands
;
_journal_issue                   5
_journal_name_full               'Chemistry Letters'
_journal_page_first              622
_journal_paper_doi               10.1246/cl.2007.622
_journal_volume                  36
_journal_year                    2007
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C13 H24 Ir O2 P S2 W '
_chemical_formula_sum            'C13 H24 Ir O2 P S2 W'
_chemical_formula_weight         683.50
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.4702(12)
_cell_length_b                   12.985(2)
_cell_length_c                   16.275(3)
_cell_measurement_reflns_used    5540
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     1790.0(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SHELXS97
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13699
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    14.197
_exptl_absorpt_correction_T_max  0.119
_exptl_absorpt_correction_T_min  0.071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1264.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.30
_refine_diff_density_min         -1.55
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1745 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.018(9)
_refine_ls_extinction_coef       4.8(14)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3664
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.0161
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[0.6700\s(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0254
_reflns_number_gt                3664
_reflns_number_total             4065
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            36-622sup1.cif
_cod_data_source_block           '__Cp*Ir(PMe3)(m-S)2W(O)2'
_cod_original_formula_sum        'C13 H24 Ir O2 P S2 W '
_cod_database_code               8000167