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_4339287
_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
'(C88 H88 Cl2 Ir2 Mo2 N8 O4 P4 2+), 2(P1 F6 1-), 2.83(C1 H2 Cl2)'
_chemical_formula_sum            'C90.83 H93.67 Cl7.66 F12 Ir2 Mo2 N8 O4 P6'
_chemical_formula_weight         2623.22
_chemical_name_systematic
; 
 ? 
;
_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                 115.3044(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.4565(4)
_cell_length_b                   12.62185(16)
_cell_length_c                   30.7539(4)
_cell_measurement_reflns_used    213951
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      32.00
_cell_measurement_theta_min      1.34
_cell_volume                     10688.0(2)
_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, 1999)'
_computing_publication_material  'SHELXL-97 and modified'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1999)'
_computing_structure_solution
'SIR97(Cascarano al.,Acta Cryst.,1996,A52,C-79)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'Rigaku R-AXIS RAPID imaging plate detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0905
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            97702
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    3.064
_exptl_absorpt_correction_T_max  0.3019
_exptl_absorpt_correction_T_min  0.2773
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Higashi, T. (1999). Shape - Program to obtain Crystal Shape using CCD
camera. Rigaku Corporation, Tokyo, Japan.
Higashi, T. (1999). Numabs - Numerical Absorption Correction, Rigaku
Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            deep-red
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5172
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.51
_refine_diff_density_max         2.075
_refine_diff_density_min         -2.564
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         12277
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0618
_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^)+(0.1082P)^2^+106.7389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1825
_refine_ls_wR_factor_ref         0.1910
_reflns_number_gt                10470
_reflns_number_total             12277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062474q-file003.cif
_cod_data_source_block           complex10
_cod_original_sg_symbol_Hall     '-C 2YC'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4339287