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_4323041
_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         ' C18 H28 P2 O2 B2 F8 '
_chemical_formula_sum            'C18 H28 B2 F8 O2 P2'
_chemical_formula_weight         255.98
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             98-06-03
_audit_creation_method           CRYSTALS
_cell_angle_alpha                90
_cell_angle_beta                 106.83(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.593(6)
_cell_length_b                   19.922(4)
_cell_length_c                   11.909(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      13.2
_cell_measurement_theta_min      13
_cell_volume                     2405.6(16)
_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)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_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  0.0087
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4613
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1
_diffrn_standards_decay_%        12.53
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.25
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psiscan
_exptl_crystal_colour            ' none '
_exptl_crystal_density_diffrn    1.41
_exptl_crystal_description       ' needle '
_exptl_crystal_F_000             1057.27
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.23
_refine_ls_extinction_coef       63.458
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   2.3113
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         2016
_refine_ls_R_factor_obs          0.0545
_refine_ls_shift/esd_max         2.289
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.0541
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_observed          2016
_reflns_number_total             4222
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ic971427i_2.cif
_cod_data_source_block           CRYSTALS_cif
_cod_original_cell_volume        2405(2)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        ' C18 H28 P2 O2 B2 F8 '
_cod_database_code               4323041