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_7024588
_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         'C262 H200 Ir16 O36 P12'
_chemical_formula_sum            'C262 H200 Ir16 O36 P12'
_chemical_formula_weight         7371.06
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2009-07-08T20:25:28-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                91.942(2)
_cell_angle_beta                 91.431(2)
_cell_angle_gamma                94.306(2)
_cell_formula_units_Z            2
_cell_length_a                   14.829(4)
_cell_length_b                   18.483(5)
_cell_length_c                   48.910(13)
_cell_measurement_reflns_used    10196
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.3
_cell_measurement_theta_min      2.25
_cell_measurement_wavelength     0.71073
_cell_volume                     13355(6)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.85
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0834
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            43138
_diffrn_reflns_theta_full        20
_diffrn_reflns_theta_max         20.58
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    8.069
_exptl_absorpt_correction_T_max  0.8616
_exptl_absorpt_correction_T_min  0.8614
_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    1.833
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6944
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.265
_refine_diff_density_min         -1.865
_refine_diff_density_rms         0.285
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1025
_refine_ls_number_reflns         23041
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0747P)^2^+731.1206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1764
_refine_ls_wR_factor_ref         0.1941
_reflns_number_gt                16576
_reflns_number_total             23041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b918770g.txt
_cod_data_source_block           b
_cod_original_cell_volume        13356(6)
_cod_database_code               7024588