Formation of Unusual Iridabenzene and Metallanaphthalene Containing Electron-Withdrawing Substituents
Margarita Paneque; Cristina M. Posadas; Manuel L. Poveda; Nuria Rendón; Verónica Salazar; Enrique Oñate; Kurt Mereiter; Journal of the American Chemical Society 125 (2003) 9898–9899; doi:10.1021/ja035655p

data_4114079
_publ_contact_author_address
;
 Instituto de Investigaciones Quimicas, C.S.I.C-Universidad de Sevilla,
 Avd. Americo Vespucio, s/n., Isla de la Cartuja, 41092 Sevilla,  Spain
;
_publ_contact_author_email       paneque@iiq.csic.es
_publ_contact_author_fax         '+34 954 460565'
_publ_contact_author_name        'Dr. Margarita Paneque'
_publ_contact_author_phone       '+34 954 489557'
_publ_section_title
;
 Formation of Unusual Iridabenzene and Metallanaphthalene Containing
 Electron-Withdrawing Substituents
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9898
_journal_page_last               9899
_journal_paper_doi               10.1021/ja035655p
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         '(C33 H40 B Ir N6 O14) (C0.25 H0.50 Cl0.5)'
_chemical_formula_sum            'C33.25 H40.5 B Cl0.5 Ir N6 O14'
_chemical_formula_weight         968.95
_chemical_name_common            'compound (4)'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.816(2)
_cell_angle_beta                 78.055(2)
_cell_angle_gamma                75.870(2)
_cell_formula_units_Z            4
_cell_length_a                   11.2272(14)
_cell_length_b                   18.882(2)
_cell_length_c                   19.527(3)
_cell_measurement_reflns_used    964
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      2
_cell_volume                     3844.0(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_detector_type            'Bruker SMART APEX'
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type
;
'three-circle diffractometer with CCD area detector'
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_sigmaI/netI    0.1469
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            46509
_diffrn_reflns_theta_full        28.53
_diffrn_reflns_theta_max         28.53
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.582
_exptl_absorpt_correction_T_max  0.769
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1938
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.083
_refine_diff_density_min         -1.237
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.782
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1021
_refine_ls_number_reflns         17776
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      0.787
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0155P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                9875
_reflns_number_total             17776
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja035655psi20030620_110237_3.cif
_cod_data_source_block           4
_cod_original_cell_volume        3844.0(8)
_cod_original_formula_sum        'C33.25 H40.50 B Cl0.50 Ir N6 O14'
_cod_database_code               4114079