Isolation of a Stable 1-Iridabicyclo[3.2.0]hepta-1,3,6-triene and Its Reversible Transformation into an Iridacycloheptatriene
Margarita Paneque; Manuel L. Poveda; Nuria Rendón; Kurt Mereiter; Journal of the American Chemical Society 126 (2004) 1610–1611; doi:10.1021/ja0393527

data_4112232
_publ_contact_author
;
Margarita Paneque 
Instituto de Investigaciones Quimicas-CSIC
Avda. Americo Vespucio s/n, Isla de la Cartuja
41092 Sevilla, SPAIN
Phone: (34)954489557
FAX:   (34)954460565
(paneque@iiq.csic.es)
;
_publ_contact_author_email       paneque@iiq.csic.es
_publ_contact_author_fax         +34-954-460565
_publ_contact_author_phone       +34-954-489557
_publ_section_title
;
 Isolation of a Stable 1-Iridabicyclo[3.2.0]hepta-1,3,6-triene and Its
 Reversible Transformation into an Iridacycloheptatriene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1610
_journal_page_last               1611
_journal_paper_doi               10.1021/ja0393527
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         '(C31 H40 B Ir N6 O8), (C H2 Cl2)'
_chemical_formula_sum            'C32 H42 B Cl2 Ir N6 O8'
_chemical_formula_weight         900.62
_chemical_name_common            'compound (4).CH2Cl2'
_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                88.743(1)
_cell_angle_beta                 75.343(1)
_cell_angle_gamma                87.515(1)
_cell_formula_units_Z            2
_cell_length_a                   11.0348(6)
_cell_length_b                   12.5531(7)
_cell_length_c                   14.0159(8)
_cell_measurement_reflns_used    6537
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      2.5
_cell_volume                     1876.43(18)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28299
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.754
_exptl_absorpt_correction_T_max  0.69
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS, V2.05'
_exptl_crystal_colour            darkgreen
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       prism
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         10785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0386P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0650
_reflns_number_gt                9696
_reflns_number_total             10785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0393527si20031216_065615_1.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4112232