Annulation of an Iridabenzene through Formal Cycloaddition Reactions with Organonitriles
Dalebrook, Andrew F.; Wright, L. James; Organometallics 28 (2009) 5536–; doi:10.1021/om900581h

data_4070041
_publ_section_title
;
 Annulation of an Iridabenzene through Formal Cycloaddition Reactions with
 Organonitriles
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              5536
_journal_paper_doi               10.1021/om900581h
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C45 H39 Cl2 F3 Ir N O3 P2 S2'
_chemical_formula_weight         1087.93
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.204(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7510(4)
_cell_length_b                   14.4940(4)
_cell_length_c                   26.2936(8)
_cell_measurement_reflns_used    9613
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      67.729
_cell_measurement_theta_min      4.921
_cell_volume                     4452.1(2)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Ortep-III (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       'Area detector \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  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            137922
_diffrn_reflns_theta_full        35.05
_diffrn_reflns_theta_max         35.05
_diffrn_reflns_theta_min         2.43
_diffrn_standards_decay_%        <2%
_exptl_absorpt_coefficient_mu    3.338
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.5827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prisms'
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.641
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         19390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+3.5021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0654
_reflns_number_gt                15892
_reflns_number_total             19389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900581h_si_002.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4070041