Functionalization of Metallabenzenes through Nucleophilic Aromatic Substitution of Hydrogen
George R. Clark; Lauren A. Ferguson; Amy E. McIntosh; Tilo Söhnel; L. James Wright; Journal of the American Chemical Society 132 (2010) 13443–13452; doi:10.1021/ja105239t

data_4103115
_publ_contact_author_address
;
Department of Chemistry
The University of Auckland
Private Bag 92019
Auckland 
New Zealand
;
_publ_contact_author_email       lj.wright@auckland.ac.nz
_publ_contact_author_fax         '0064 9 3737422'
_publ_contact_author_name        'Wright, L. James'
_publ_contact_author_phone       '0064 9 3737599 Ext 88257'
_publ_section_title
;
 Functionalization of Metallabenzenes through Nucleophilic Aromatic
 Substitution of Hydrogen
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13443
_journal_page_last               13452
_journal_paper_doi               10.1021/ja105239t
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C48 H49 Ir N P2 S3 , C2 H4 Cl2 , F6 P'
_chemical_formula_sum            'C50 H53 Cl2 F6 Ir N P3 S3'
_chemical_formula_weight         1234.12
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.6490(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8600(3)
_cell_length_b                   21.6582(5)
_cell_length_c                   19.9376(5)
_cell_measurement_reflns_used    8217
_cell_measurement_temperature    89(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.99
_cell_volume                     5015.8(2)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_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      89(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Siemens SMART 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  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            63733
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.40
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.048
_exptl_absorpt_correction_T_max  0.7926
_exptl_absorpt_correction_T_min  0.4824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.573
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         11847
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+4.1096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0688
_reflns_number_gt                9353
_reflns_number_total             11847
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja105239t_si_003_4.cif
_cod_data_source_block           Compound_6
_cod_original_sg_symbol_Hall     -p_2yn
_cod_database_code               4103115