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_4336223
_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_absolute_configuration ad
_chemical_formula_moiety         'C29 H25 Ir3 Mo2 O9, C H Cl3'
_chemical_formula_sum            'C30 H26 Cl3 Ir3 Mo2 O9'
_chemical_formula_weight         1405.43
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6450(2)
_cell_length_b                   12.4173(2)
_cell_length_c                   26.4766(4)
_cell_measurement_reflns_used    150817
_cell_measurement_temperature    200
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     3499.73(10)
_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 0.996
_diffrn_measured_fraction_theta_max 0.994
_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  0.098
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            53459
_diffrn_reflns_theta_full        29.491
_diffrn_reflns_theta_max         30.093
_diffrn_reflns_theta_min         2.832
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.342
_exptl_absorpt_correction_T_max  0.616
_exptl_absorpt_correction_T_min  0.171
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.667
_exptl_crystal_description       plate
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.040
_refine_diff_density_max         3.28
_refine_diff_density_min         -2.44
_refine_ls_abs_structure_details 'Flack (1983), 4474 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.011(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9848
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         5701
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.0010306
_refine_ls_shift/su_mean         0.0000237
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ +12.30P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0745
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0745
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              37
_reflns_limit_l_min              0
_reflns_number_gt                4474
_reflns_number_total             5701
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.23
_oxford_diffrn_Wilson_scale      181.11
_oxford_refine_ls_r_factor_ref   0.0423
_oxford_refine_ls_scale          0.106832(18)
_oxford_reflns_number_all        5700
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            ic401502f_si_002_06.cif
_cod_data_source_block           3a
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               4336223