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_4336221
_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         'C24 H18 Ir4 O10 W1'
_chemical_formula_sum            'C24 H18 Ir4 O10 W'
_chemical_formula_weight         1419.13
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             12-08-22
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                90
_cell_angle_beta                 109.0795(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7438(3)
_cell_length_b                   8.95740(10)
_cell_length_c                   19.3271(3)
_cell_measurement_reflns_used    34501
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     2739.46(7)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans with CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.085
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            59136
_diffrn_reflns_theta_full        27.498
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.574
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.598
_exptl_absorpt_correction_T_max  0.565
_exptl_absorpt_correction_T_min  0.058
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    3.441
_exptl_crystal_description       lath
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.91
_refine_diff_density_min         -1.86
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9763
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6281
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.0010327
_refine_ls_shift/su_mean         0.0000374
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 6.13P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0659
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0659
_reflns_limit_h_max              20
_reflns_limit_h_min              -21
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                5243
_reflns_number_total             6281
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.85
_oxford_diffrn_Wilson_scale      625.15
_oxford_refine_ls_r_factor_ref   0.0405
_oxford_refine_ls_scale          0.066521(8)
_oxford_reflns_number_all        6281
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            ic401502f_si_002_04.cif
_cod_data_source_block           1d
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C24 H18 Ir4 O10 W1'
_cod_database_code               4336221