Rhodium and Iridium Hydroxide Complexes [M(μ-OH)(COD)]2(M = Rh, Ir) as Versatile Precursors of Homo and Early−Late Heterobimetallic Compounds. X-ray Crystal Structures of Cp*Ta(μ3-O)4[Rh(COD)]4(Cp* = η5-C5Me5) and [Ir(2-O-3-CN-4,6-Me2-C5HN)(COD)]2
Fandos, Rosa; Hernández, Carolina; Otero, Antonio; Rodríguez, Ana; Ruiz, Maria José; García Fierro, José Luis; Terreros, Pilar; Organometallics 18 (1999) 2718–; doi:10.1021/om990065e

data_4077762
_publ_section_title
;
 Rhodium and Iridium Hydroxide Complexes [M(\m-OH)(COD)]2(M = Rh, Ir) as
 Versatile Precursors of Homo and Early&#x2212;Late Heterobimetallic
 Compounds. X-ray Crystal Structures of Cp*Ta(\m3-O)4[Rh(COD)]4(Cp* =
 \h5-C5Me5) and [Ir(2-O-3-CN-4,6-Me2-C5HN)(COD)]2
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              2718
_journal_paper_doi               10.1021/om990065e
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C32 H38 Ir2 N4 O2'
_chemical_formula_weight         895.06
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.76(5)
_cell_angle_beta                 70.11(4)
_cell_angle_gamma                61.37(2)
_cell_formula_units_Z            2
_cell_length_a                   10.561(4)
_cell_length_b                   10.988(3)
_cell_length_c                   15.450(10)
_cell_measurement_reflns_used    2
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     1479.8(13)
_computing_cell_refinement       'MACH3 (Nonius)'
_computing_data_collection       'MACH3 (Nonius)'
_computing_data_reduction        'XRAY80 (Stewart,1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'four circle diffractometer, Nonius-MAch3'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7134
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    9.020
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.473
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.510
_refine_diff_density_min         -4.766
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7134
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1221
_reflns_number_gt                5096
_reflns_number_total             7134
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om990065e.cif
_cod_data_source_block           8
_cod_original_cell_volume        1479.8(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077762