Synthesis and X-ray crystal structure of a novel organometallic (μ3-oxido)(μ3-imido) trinuclear iridium complex.
Schau-Magnussen, Magnus; Malcho, Phillip; Herbst, Konrad; Brorson, Michael; Bendix, Jesper; Dalton transactions (Cambridge, England : 2003) 40 (2011) 4212–4216; doi:10.1039/c0dt01791d

data_7015646
_publ_section_title
;
 Synthesis and X-ray crystal structure of a novel organometallic
 (\m3-oxido)(\m3-imido) trinuclear iridium complex.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4212
_journal_page_last               4216
_journal_paper_doi               10.1039/c0dt01791d
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C34 H54 Ir3 N O, 2(C F3 O3 S)'
_chemical_formula_sum            'C36 H54 F6 Ir3 N O7 S2'
_chemical_formula_weight         1367.52
_chemical_name_common
;
((mu!3$-imido)(mu!3$-oxo)tris(eta$5!-
pentamethylcyclopentadienyliridium(iii))) triflate
;
_chemical_name_systematic
;
[(\m~3~-imido)(\m~3~-oxo)tris(\h^5^-pentamethylcyclopentadienyliridium(iii))]
triflate
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 93.085(9)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   21.5130(8)
_cell_length_b                   13.535(3)
_cell_length_c                   14.3094(14)
_cell_measurement_reflns_used    29157
_cell_measurement_temperature    122(1)
_cell_measurement_theta_max      34.16
_cell_measurement_theta_min      1.43
_cell_volume                     4160.6(10)
_computing_cell_refinement       'COLLECT (Nonius, 1999)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EvalCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      122(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\w and \f 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  0.1180
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48722
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    9.746
_exptl_absorpt_correction_T_max  0.315
_exptl_absorpt_correction_T_min  0.065
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    2.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.894
_refine_diff_density_min         -2.450
_refine_diff_density_rms         0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         4991
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0291
_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^)+(0.0386P)^2^+4.0274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0826
_reflns_number_gt                4440
_reflns_number_total             4991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01791d.txt
_cod_data_source_block           (2)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7015646