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_4103112
_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         'C49 H51 Ir N O P2 S3, P F6'
_chemical_formula_sum            'C49 H51 F6 Ir N O P3 S3'
_chemical_formula_weight         1165.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           1
_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                102.787(1)
_cell_angle_beta                 93.846(1)
_cell_angle_gamma                90.24
_cell_formula_units_Z            1
_cell_length_a                   10.3592(2)
_cell_length_b                   10.4724(2)
_cell_length_c                   11.3705(1)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    84(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      1.99
_cell_volume                     1200.01(3)
_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      84(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0758
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11614
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.074
_exptl_absorpt_correction_T_max  0.668290
_exptl_absorpt_correction_T_min  0.547541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.555
_refine_diff_density_min         -3.481
_refine_diff_density_rms         0.202
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         8877
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          1.789
_refine_ls_shift/su_mean         0.035
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0928P)^2^+5.5832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1542
_reflns_number_gt                8724
_reflns_number_total             8877
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja105239t_si_003_1.cif
_cod_data_source_block           Compound_7
_cod_original_cell_volume        1200.00(3)
_cod_original_sg_symbol_Hall     p_1
_cod_database_code               4103112