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_4060817
_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_sum            'C30 H48 Cl Ir3 S4'
_chemical_formula_weight         1149.06
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_audit_creation_date             'Fri Aug 17 02:34:23 2001'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.894(2)
_cell_length_b                   19.736(3)
_cell_length_c                   18.098(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      19.9
_cell_measurement_theta_min      19.0
_cell_volume                     3533(1)
_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  teXsan
_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      0.09973
_diffrn_orient_matrix_UB_12      0.00739
_diffrn_orient_matrix_UB_13      -0.00395
_diffrn_orient_matrix_UB_21      -0.01442
_diffrn_orient_matrix_UB_22      0.05009
_diffrn_orient_matrix_UB_23      0.00262
_diffrn_orient_matrix_UB_31      0.00784
_diffrn_orient_matrix_UB_32      -0.00185
_diffrn_orient_matrix_UB_33      0.05505
_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  1.066
_diffrn_reflns_av_sigmaI/netI    0.070
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4182
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        2.38
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.631
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.160
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2160.00
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.99
_refine_diff_density_min         -1.04
_refine_ls_extinction_coef       0.00060(6)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.298
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2718
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.0020
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00014|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0340
_refine_ls_wR_factor_ref         0.0340
_reflns_number_gt                2718
_reflns_number_total             4181
_reflns_threshold_expression     >3.0sigma(I)
_cod_database_code               4060817