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_4060816
_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            'C33 H50 Ir3 S4'
_chemical_formula_weight         1151.66
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_audit_creation_date             'Fri Oct 13 03:26:00 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 122.465(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.522(2)
_cell_length_b                   19.011(2)
_cell_length_c                   12.912(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                     3628.8(7)
_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      -0.04583
_diffrn_orient_matrix_UB_12      -0.03793
_diffrn_orient_matrix_UB_13      -0.02219
_diffrn_orient_matrix_UB_21      -0.01769
_diffrn_orient_matrix_UB_22      0.02209
_diffrn_orient_matrix_UB_23      0.05442
_diffrn_orient_matrix_UB_31      -0.04650
_diffrn_orient_matrix_UB_32      0.02899
_diffrn_orient_matrix_UB_33      -0.07051
_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  0.032
_diffrn_reflns_av_sigmaI/netI    0.054
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4432
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.76
_diffrn_standards_decay_%        -10.52
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.256
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.276
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            darkred
_exptl_crystal_density_diffrn    2.108
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2172.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.49
_refine_diff_density_min         -3.75
_refine_ls_extinction_coef       0.0012(1)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.944
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     143
_refine_ls_number_reflns         3101
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.2390
_refine_ls_shift/su_mean         0.0250
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00027|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0588
_reflns_number_gt                3101
_reflns_number_total             4295
_reflns_threshold_expression     >3.0sigma(I)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4060816