Regioselective Phosphine Addition to [(η5-C5Me5)Ir(η5-oxocyclohexadienyl)]+ and X-ray Structure of the Stable Phenol Tautomer Complex [(η5-C5Me5)Ir(η4-exo-2-(PMe3)C6H5O)]+: A Key Intermediate for the Nucleophilic Phenol Functionalization Reaction
J. Le Bras; H. Amouri; J. Vaissermann; Inorganic Chemistry 37 (1998) 5056–5060; doi:10.1021/ic971427i

data_4323042
_publ_contact_author
;
 Dr H. Amouri, E.N.S.C.P., 11, rue P. et M. Curie, 75231 Paris Cedex 05, France
;
_publ_contact_author_fax         ' (33) 1 43 25 79 75 '
_publ_contact_author_phone       ' (33) 1 44 27 66 99 '
_publ_section_title
;
 Regioselective Phosphine Addition to
 [(\h5-C5Me5)Ir(\h5-oxocyclohexadienyl)]+ and X-ray Structure of the
 Stable Phenol Tautomer Complex [(\h5-C5Me5)Ir(\h4-exo-2-(PMe3)C6H5O)]+: A
 Key Intermediate for the Nucleophilic Phenol Functionalization Reaction
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5056
_journal_page_last               5060
_journal_paper_doi               10.1021/ic971427i
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C20 H0 Ir2 I6 '
_chemical_formula_sum            'C20 H0 I6 Ir2'
_chemical_formula_weight         1416.3
_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_primary     direct
_audit_creation_date             98-06-03
_audit_creation_method           CRYSTALS
_cell_angle_alpha                90
_cell_angle_beta                 100.89(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.533(3)
_cell_length_b                   8.374(1)
_cell_length_c                   23.541(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      14.3
_cell_measurement_theta_min      14
_cell_volume                     3006.9(9)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
;
RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)
;
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_diffrn_ambient_temperature      295
_diffrn_measurement_device       '  Enraf-nonius CAD4 '
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            5882
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1
_diffrn_standards_decay_%        3.63
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    14.92
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            ' dark brown '
_exptl_crystal_density_diffrn    3.13
_exptl_crystal_description       ' prism '
_exptl_crystal_F_000             2333.77
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.68
_refine_diff_density_min         -1.42
_refine_ls_extinction_coef       86.1(43)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   1.1389
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4047
_refine_ls_R_factor_obs          0.0364
_refine_ls_shift/esd_max         2.07988
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.0443
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_observed          4047
_reflns_number_total             5257
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ic971427i_3.cif
_cod_data_source_block           CRYSTALS_cif
_cod_original_cell_volume        3006.6(9)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        ' C20 H0 Ir2 I6 '
_cod_database_code               4323042