Syntheses of Pentanuclear Group 6 Iridium Clusters by Core Expansion of Tetranuclear Clusters with Ir(CO)2(η5-C5Me4R) (R = H, Me)
Michael D. Randles; Peter V. Simpson; Vivek Gupta; Junhong Fu; Graeme J. Moxey; Torsten Schwich; Alan L. Criddle; Simon Petrie; Jonathan G. MacLellan; Stuart R. Batten; Robert Stranger; Marie P. Cifuentes; Mark G. Humphrey; Inorganic Chemistry 52 (2013) 11256–11268; doi:10.1021/ic401502f

data_4336225
_publ_section_title
;
 Syntheses of Pentanuclear Group 6 Iridium Clusters by Core Expansion of
 Tetranuclear Clusters with Ir(CO)2(\h5-C5Me4R) (R = H, Me)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11256
_journal_page_last               11268
_journal_paper_doi               10.1021/ic401502f
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C28 H23 Ir3 Mo2 O9'
_chemical_formula_sum            'C28 H23 Ir3 Mo2 O9'
_chemical_formula_weight         1271.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_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                 93.595(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0292(11)
_cell_length_b                   20.408(2)
_cell_length_c                   13.8617(16)
_cell_measurement_reflns_used    35249
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.12
_cell_measurement_theta_min      3.15
_cell_volume                     2831.6(5)
_computing_cell_refinement       'Bruker Apex2 v2.0 (Bruker Axs 2005)'
_computing_data_collection       'Bruker Apex2 v2.0 (Bruker Axs 2005)'
_computing_data_reduction        'Bruker Apex2 v2.0 (Bruker Axs 2005)'
_computing_molecular_graphics    'X-seed (Barbour, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker X8 Apex KAPPA CCD'
_diffrn_measurement_method       '0.5 deg frames in phi and omega'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34631
_diffrn_reflns_theta_full        30.10
_diffrn_reflns_theta_max         30.10
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    14.964
_exptl_absorpt_correction_T_max  0.3161
_exptl_absorpt_correction_T_min  0.1538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.984
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.769
_refine_diff_density_min         -2.373
_refine_diff_density_rms         0.618
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         8172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0461P)^2^+2.5635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.1043
_reflns_number_gt                6947
_reflns_number_total             8172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401502f_si_002_08.cif
_cod_data_source_block           3c
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4336225