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_8000169
_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         'C52 H65 Cl Ir N2 P S W '
_chemical_formula_sum            'C52 H65 Cl Ir N2 P S W'
_chemical_formula_weight         1192.66
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   21.684(3)
_cell_length_b                   12.9161(19)
_cell_length_c                   17.115(3)
_cell_measurement_reflns_used    14766
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     4793.4(13)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.059
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            34880
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    5.351
_exptl_absorpt_correction_T_max  0.201
_exptl_absorpt_correction_T_min  0.066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2360.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         5.86
_refine_diff_density_min         -3.15
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  4104 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.004(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     592
_refine_ls_number_reflns         8191
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.0032
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[1.1000\s(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0359
_reflns_number_gt                8191
_reflns_number_total             9761
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            36-622sup1.cif
_cod_data_source_block           '__Cp*IrH(PPh3)(m-S)WCl(NAr)2'
_cod_original_cell_volume        4793.3(12)
_cod_original_formula_sum        'C52 H65 Cl Ir N2 P S W '
_cod_database_code               8000169