Linear metal-metal-bonded tetranuclear M-Mo-Mo-M complexes (M = Ir and Rh): oxidative metal-metal bond formation in a tetrametallic system and 1,4-addition reaction of alkyl halides.
Ohashi, Masato; Shima, Asuka; Rüffer, Tobias; Mizomoto, Hitoshi; Kaneda, Yutaka; Mashima, Kazushi; Inorganic chemistry 46 (2007) 6702–6714; doi:10.1021/ic062474q

data_4339288
_publ_section_title
;
 Linear metal-metal-bonded tetranuclear M-Mo-Mo-M complexes (M = Ir and
 Rh): oxidative metal-metal bond formation in a tetrametallic system and
 1,4-addition reaction of alkyl halides.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6702
_journal_page_last               6714
_journal_paper_doi               10.1021/ic062474q
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety
'(C104 H88 I2 Ir2 Mo2 N8 O4 P4 2+), 2(B C24 H20 1-), 3(C2 H4 Cl2), 2(H2 O)'
_chemical_formula_sum            'C158 H144 B2 Cl6 I2 Ir2 Mo2 N8 O6 P4'
_chemical_formula_weight         3439.09
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 126.749(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   33.885(3)
_cell_length_b                   19.787(3)
_cell_length_c                   27.629(3)
_cell_measurement_reflns_used    75045
_cell_measurement_temperature    114(1)
_cell_measurement_theta_max      30.99
_cell_measurement_theta_min      2.99
_cell_volume                     14843(3)
_computing_cell_refinement       'Rigaku/RAPID Diffractometer Control'
_computing_data_collection       'Rigaku/RAPID Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_molecular_graphics    'Ortep-3 (Louis J. Farrugia, 2005)'
_computing_publication_material  'SHELXL-97 and modified'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      114(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_details
;
RAPID: Eulerian 3-circle
;
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_collimation    ' 0.8 mm double pinhole '
_diffrn_radiation_detector       'imaging plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1107
_diffrn_reflns_av_sigmaI/netI    0.0738
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            146593
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.99
_diffrn_source_current           40
_diffrn_source_power             50
_exptl_absorpt_coefficient_mu    2.577
_exptl_absorpt_correction_T_max  0.7697
_exptl_absorpt_correction_T_min  0.4836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). ABSCOR - Program for Absorption Correction, Rigaku
        Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            ' red '
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ' needle '
_exptl_crystal_F_000             6848
_exptl_crystal_preparation
'mounted on the CryoLoop with mineral oil and placed in N2 stream at 114(1) K'
_exptl_crystal_recrystallization_method
'crystallization from a solution of CH2ClCH2Cl/ether at ambient temperature'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.866
_refine_diff_density_min         -2.927
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     877
_refine_ls_number_reflns         22576
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0774P)^2^+108.6094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1691
_reflns_number_gt                14520
_reflns_number_total             22576
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062474q-file003.cif
_cod_data_source_block           complex12
_cod_original_sg_symbol_Hall     ' -C 2yc '
_cod_original_sg_symbol_H-M      ' C 2/c '
_cod_database_code               4339288