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_4323040
_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         ' C19 H29 Ir1 P1 O1 B1 F4 '
_chemical_formula_sum            'C19 H29 B F4 Ir O P'
_chemical_formula_weight         583.44
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             98-06-03
_audit_creation_method           CRYSTALS
_cell_angle_alpha                95.90(1)
_cell_angle_beta                 99.47(1)
_cell_angle_gamma                99.20(1)
_cell_formula_units_Z            2
_cell_length_a                   8.599(1)
_cell_length_b                   9.0173(9)
_cell_length_c                   14.448(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      15.2
_cell_measurement_theta_min      15
_cell_volume                     1081.2(3)
_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  0.015
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4081
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1
_diffrn_standards_decay_%        43.14
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    6.26
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   DIFABS
_exptl_absorpt_process_details   'refined from delta-F'
_exptl_crystal_colour            ' off white '
_exptl_crystal_density_diffrn    1.79
_exptl_crystal_description       ' prism '
_exptl_crystal_F_000             564.11
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.80
_refine_diff_density_min         -2.68
_refine_ls_extinction_coef       40.4(30)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   4.8034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3304
_refine_ls_R_factor_obs          0.0444
_refine_ls_shift/esd_max         1.76
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.0519
_reflns_limit_h_max              9
_reflns_limit_h_min              -10
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_observed          3304
_reflns_number_total             3803
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ic971427i_1.cif
_cod_data_source_block           CRYSTALS_cif
_cod_original_cell_volume        1081.1(3)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C19 H29 Ir1 P1 O1 B1 F4 '
_cod_database_code               4323040