Synthesis and Characterization of [Ir(1,5-Cyclooctadiene)(μ-H)]4: A Tetrametallic Ir4H4- Core, Coordinatively Unsaturated Cluster
Kuang-Hway Yih; Isil K. Hamdemir; Joseph E. Mondloch; Ercan Bayram; Saim Özkar; Relja Vasić; Anatoly I. Frenkel; Oren P. Anderson; Richard G. Finke; Inorganic Chemistry 51 (2012) 3186–3193; doi:10.1021/ic2026494

data_4328566
_publ_section_title
;
 Synthesis and Characterization of [Ir(1,5-Cyclooctadiene)(\m-H)]4: A
 Tetrametallic Ir4H4- Core, Coordinatively Unsaturated Cluster
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3186
_journal_page_last               3193
_journal_paper_doi               10.1021/ic2026494
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C32 H52 Ir4'
_chemical_formula_weight         1205.54
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2011-06-29 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5628(3)
_cell_length_b                   18.4647(5)
_cell_length_c                   12.3963(3)
_cell_measurement_reflns_used    9584
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.16
_cell_measurement_theta_min      2.56
_cell_volume                     2875.55(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            74947
_diffrn_reflns_theta_full        33.17
_diffrn_reflns_theta_max         33.17
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    18.473
_exptl_absorpt_correction_T_max  0.3196
_exptl_absorpt_correction_T_min  0.3196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.785
_exptl_crystal_description       prism
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.228
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         5503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0151
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0092P)^2^+5.2247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0312
_refine_ls_wR_factor_ref         0.0319
_reflns_number_gt                5061
_reflns_number_total             5503
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2026494_si_002.cif
_cod_data_source_block           rf118
_cod_database_code               4328566