Four tetrairidium carbonyl clusters linked by six diphosphino ligands: synthesis and X-ray structure of [{Ir(4)(CO)(9)}(4)(dppmb)(6)] (dppmb = 1,4-bis(diphenylphosphinomethyl)benzene.
Peli, Giulia; Daghetta, Matteo; Macchi, Piero; Sironi, Angelo; Garlaschelli, Luigi; Dalton transactions (Cambridge, England : 2003) 39 (2010) 1188–1190; doi:10.1039/b918770g

data_7024587
_publ_section_title
;
 Four tetrairidium carbonyl clusters linked by six diphosphino ligands:
 synthesis and X-ray structure of [{Ir(4)(CO)(9)}(4)(dppmb)(6)] (dppmb =
 1,4-bis(diphenylphosphinomethyl)benzene.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1188
_journal_page_last               1190
_journal_paper_doi               10.1039/b918770g
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C242 H184 Ir16 O36 P12'
_chemical_formula_sum            'C242 H184 Ir16 O36 P12'
_chemical_formula_weight         7114.73
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-07-08T19:15:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.9060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.8355(18)
_cell_length_b                   14.9833(14)
_cell_length_c                   49.076(5)
_cell_measurement_reflns_used    8838
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      23.5
_cell_measurement_theta_min      2.3
_cell_measurement_wavelength     0.71073
_cell_volume                     13842(2)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.919
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1185
_diffrn_reflns_av_unetI/netI     0.146
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            126773
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         29.71
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    7.782
_exptl_absorpt_correction_T_max  0.2105
_exptl_absorpt_correction_T_min  0.1871
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6672
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.025
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1151
_refine_ls_number_reflns         36149
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1846
_refine_ls_R_factor_gt           0.0775
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+34.9184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1751
_refine_ls_wR_factor_ref         0.2177
_reflns_number_gt                16837
_reflns_number_total             36149
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b918770g.txt
_cod_data_source_block           a
_cod_original_cell_volume        13843(2)
_cod_database_code               7024587