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_4077761
_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            'C42 H63 O4 Rh4 Ta'
_chemical_formula_weight         1224.51
_chemical_name_systematic
; 
 ? 
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.630(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.678(5)
_cell_length_b                   11.5590(10)
_cell_length_c                   20.4740(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     4065.8(12)
_computing_cell_refinement       'Nonius  (control program)'
_computing_data_collection       'Nonius (control program)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'four circle diffractometer Nonius-Mach3'
_diffrn_measurement_method       '\w/2\2q 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    0.1522
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            9778
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        4
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.310
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.782
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.000
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.387
_refine_diff_density_min         -1.699
_refine_diff_density_rms         0.297
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         9778
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1490
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.1407
_reflns_number_gt                4411
_reflns_number_total             9778
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om990065e.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      P2(1(/n
_cod_database_code               4077761