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_4336227
_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 O9 W2'
_chemical_formula_sum            'C28 H23 Ir3 O9 W2'
_chemical_formula_weight         1447.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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                 103.83(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.553(2)
_cell_length_b                   16.679(3)
_cell_length_c                   16.864(3)
_cell_measurement_reflns_used    11273
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.74
_cell_volume                     2882.2(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    Olex2
_computing_publication_material  'Microsoft Office 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'psi and omega scans'
_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  0.0778
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49243
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    21.806
_exptl_absorpt_correction_T_max  1.178
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.336
_exptl_crystal_description       block
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         7.379
_refine_diff_density_min         -4.336
_refine_diff_density_rms         0.642
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         6614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0571
_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^)+(0.1094P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1413
_refine_ls_wR_factor_ref         0.1483
_reflns_number_gt                5499
_reflns_number_total             6614
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401502f_si_002_10.cif
_cod_data_source_block           4
_cod_original_cell_volume        2882.3(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4336227