Synthesis of a New Tetrakis(hydrosulfido) Diiridium Complex and Its Conversion into Homo- and Heterometallic Sulfido-Hydrosulfido Clusters
Takagi, Fusao; Seino, Hidetake; Mizobe, Yasushi; Hidai, Masanobu; Organometallics 21 (2002) 694–699; doi:10.1021/om0108550

data_4060815
_publ_section_title
;
Synthesis of a New Tetrakis(hydrosulfido) Diiridium Complex and Its 
Conversion into Homo- and Heterometallic Sulfido-Hydrosulfido Clusters
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              694
_journal_page_last               699
_journal_paper_doi               10.1021/om0108550
_journal_volume                  21
_journal_year                    2002
_chemical_formula_moiety         'C20 H34 Ir2 S4'
_chemical_formula_sum            'C20 H34 Ir2 S4'
_chemical_formula_weight         787.17
_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'
_audit_creation_date             'Wed Oct 11 19:19:01 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 104.125(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.588(1)
_cell_length_b                   9.3975(9)
_cell_length_c                   15.728(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      19.1
_cell_volume                     1231.0(2)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  SHELXL97
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.01492
_diffrn_orient_matrix_UB_12      -0.03746
_diffrn_orient_matrix_UB_13      -0.06097
_diffrn_orient_matrix_UB_21      0.01827
_diffrn_orient_matrix_UB_22      -0.09903
_diffrn_orient_matrix_UB_23      0.02359
_diffrn_orient_matrix_UB_31      -0.11773
_diffrn_orient_matrix_UB_32      -0.01062
_diffrn_orient_matrix_UB_33      -0.00493
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_av_sigmaI/netI    0.032
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2318
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.00
_diffrn_standards_decay_%        0.88
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.172
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.259
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.124
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             744.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         3.80
_refine_diff_density_min         -3.94
_refine_diff_density_rms         0.36
_refine_ls_extinction_coef       0.0065
_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   1.026
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          -0.0750
_refine_ls_shift/su_mean         0.0040
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.1384P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1668
_reflns_number_gt                1828
_reflns_number_total             2163
_reflns_threshold_expression     >2.0sigma(I)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4060815