η6-Tetramethylfulvene and μ-η3:η3-Benzene Complexes of Iridium
Meredith, Joseph M.; Goldberg, Karen I.; Kaminsky, Werner; Heinekey, D. Michael; Organometallics 31 (2012) 8459–; doi:10.1021/om3010492

data_4079735
_publ_section_title
;
 \h6-Tetramethylfulvene and \m-\h3:\h3-Benzene Complexes of Iridium
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              8459
_journal_paper_doi               10.1021/om3010492
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C17 H28 Ir N2, C24 B F20'
_chemical_formula_sum            'C41 H28 B F20 Ir N2'
_chemical_formula_weight         1131.66
_chemical_name_common            JMM02051
_chemical_name_systematic        JMM02051
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 104.7847(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9124(4)
_cell_length_b                   15.2581(4)
_cell_length_c                   18.9291(7)
_cell_measurement_reflns_used    794
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     3885.2(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w 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  0.0861
_diffrn_reflns_av_sigmaI/netI    0.1605
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15952
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    3.569
_exptl_absorpt_correction_T_max  0.5659
_exptl_absorpt_correction_T_min  0.4140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2008
_exptl_crystal_colour            pale-brown
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.323
_refine_diff_density_min         -1.281
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         9228
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.853
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0802
_reflns_number_gt                5267
_reflns_number_total             9228
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3010492_si_001.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4079735