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_4336222
_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         'C29 H30 Ir4 Mo1 O9'
_chemical_formula_sum            'C29 H30 Ir4 Mo O9'
_chemical_formula_weight         1387.37
_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
_audit_creation_date             12-08-30
_audit_creation_method           CRYSTALS_ver_14.05
_cell_angle_alpha                90
_cell_angle_beta                 99.3334(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0021(3)
_cell_length_b                   18.1098(5)
_cell_length_c                   16.2304(4)
_cell_measurement_reflns_used    25409
_cell_measurement_temperature    200
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     3191.03(15)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.138
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            50292
_diffrn_reflns_theta_full        22.466
_diffrn_reflns_theta_max         22.466
_diffrn_reflns_theta_min         2.584
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.053
_exptl_absorpt_correction_T_max  0.662
_exptl_absorpt_correction_T_min  0.188
_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    2.888
_exptl_crystal_description       plate
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.14
_refine_diff_density_min         -2.27
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9366
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         4134
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.0153030
_refine_ls_shift/su_mean         0.7394134
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 5.86 8.60 4.41 1.24 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0895
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0895
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                3180
_reflns_number_total             4153
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.40
_oxford_diffrn_Wilson_scale      2315.84
_oxford_refine_ls_r_factor_ref   0.0525
_oxford_refine_ls_scale          0.030022(3)
_oxford_reflns_number_all        4134
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            ic401502f_si_002_05.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C29 H30 Ir4 Mo1 O9'
_cod_database_code               4336222