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_4103114
_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         'C47 H44 Ir N P2 S3'
_chemical_formula_sum            'C47 H44 Ir N P2 S3'
_chemical_formula_weight         973.15
_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                90.000
_cell_angle_beta                 96.557(4)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   17.8209(10)
_cell_length_b                   10.1255(6)
_cell_length_c                   23.1175(12)
_cell_measurement_reflns_used    8969
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      1.77
_cell_volume                     4144.2(4)
_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      90(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0726
_diffrn_reflns_av_sigmaI/netI    0.2387
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            66483
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.485
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.005
_refine_diff_density_max         2.304
_refine_diff_density_min         -2.195
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         9909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.2008
_refine_ls_R_factor_gt           0.0791
_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^)+(0.0685P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1816
_reflns_number_gt                4535
_reflns_number_total             9909
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja105239t_si_003_3.cif
_cod_data_source_block           Compound_3
_cod_original_sg_symbol_Hall     -p_2ybc
_cod_database_code               4103114