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_4113455
_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         'C33 H38 B Ir N6 O9'
_chemical_formula_sum            'C33 H38 B Ir N6 O9'
_chemical_formula_weight         865.70
_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                74.638(2)
_cell_angle_beta                 86.425(2)
_cell_angle_gamma                81.588(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6037(9)
_cell_length_b                   12.1858(9)
_cell_length_c                   12.9590(10)
_cell_measurement_reflns_used    7624
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.98
_cell_measurement_theta_min      2.318
_cell_volume                     1747.4(2)
_computing_cell_refinement       'SAINT+ v. 6.04 (Bruker-AXS, 2001)'
_computing_data_collection       'SMART v. 5.625 (Bruker-AXS, 2001)'
_computing_data_reduction        'SAINT+ v. 6.04 (Bruker-AXS, 2001)'
_computing_molecular_graphics    'xp program, SHELXTL v. 6.10, BRUKER, 2000'
_computing_publication_material  'XCIF program, SHELXTL v. 6.10, Bruker, 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 8.53
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART 6000 CCD system'
_diffrn_measurement_method       'phi and omega 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  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12520
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.02
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.882
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.3354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS v. 2.03: Area-Detector Absorption Correction.
 (1997-2001) Bruker-AXS within SAINT+ package, v. 6.04
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.848
_refine_diff_density_min         -1.501
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         7571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          2.637
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0687
_reflns_number_gt                6805
_reflns_number_total             7571
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0290375-3_s1_5.cif
_cod_data_source_block           6
_cod_database_code               4113455