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_4113451
_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           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.0720(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9871(5)
_cell_length_b                   21.0604(14)
_cell_length_c                   21.0566(14)
_cell_measurement_reflns_used    7770
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.31
_cell_measurement_theta_min      2.16
_cell_volume                     3528.1(4)
_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      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker Smart APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40068
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.846
_exptl_absorpt_correction_T_max  0.8645
_exptl_absorpt_correction_T_min  0.4823
_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    1.630
_exptl_crystal_description       plate
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.397
_refine_diff_density_min         -1.304
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         8455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                6438
_reflns_number_total             8455
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0290375-3_s1_1.cif
_cod_data_source_block           7
_cod_database_code               4113451