Coupling of Internal Alkynes in TpMe2Ir Derivatives: Selective Oxidation of a Noncoordinated Double Bond of the Resulting Iridacycloheptatrienes
Eleuterio Álvarez; Margarita Gómez; Margarita Paneque; Cristina M. Posadas; Manuel L. Poveda; Nuria Rendón; Laura L. Santos; Susana Rojas-Lima; Verónica Salazar; Kurt Mereiter; Caridad Ruiz; Journal of the American Chemical Society 125 (2003) 1478–1479; doi:10.1021/ja0290375

data_4113453
_publ_contact_author_address
;
 Dr. Margarita Paneque
 Instituto de Investigaciones Qu\'imicas, C.S.I.C-Universidad de Sevilla,
 Avd. Am\'erico Vespucio, s/n., Isla de la Cartuja, 41092 Sevilla,  Spain
;
_publ_contact_author_email       paneque@iiq.csic.es
_publ_contact_author_fax         '+34 954 460565'
_publ_contact_author_name        'Dr. Margarita Paneque'
_publ_contact_author_phone       '+34 954 489557'
_publ_section_title
;
 Coupling of Internal Alkynes in TpMe2Ir Derivatives: Selective Oxidation
 of a Noncoordinated Double Bond of the Resulting Iridacycloheptatrienes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1478
_journal_page_last               1479
_journal_paper_doi               10.1021/ja0290375
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C29 H38 B Ir N6 O8'
_chemical_formula_sum            'C29 H38 B Ir N6 O8'
_chemical_formula_weight         801.66
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.541(3)
_cell_angle_beta                 85.535(3)
_cell_angle_gamma                64.231(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0964(15)
_cell_length_b                   10.9412(16)
_cell_length_c                   15.692(2)
_cell_measurement_reflns_used    1004
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.6
_cell_volume                     1543.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker Smart CCD'
_diffrn_measurement_method       '\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  0.0187
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27579
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    4.384
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;  
  Correction for absorption, crystal decay (insignificant) and effects of 
  the CCD detector by semi-empirical method from equivalents using program 
  SADABS (G.M. Sheldrick, 1996, Univ. of Goettingen, Germany).
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       'prism '
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.856
_refine_diff_density_min         -1.382
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.00074(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         8747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+1.7952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0528
_reflns_number_gt                8303
_reflns_number_total             8747
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0290375-3_s1_3.cif
_cod_data_source_block           2
_cod_database_code               4113453