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_4112233
_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         '(C27 H36 B Ir N6 O9), 1.25(H2 O)'
_chemical_formula_sum            'C27 H38.5 B Ir N6 O10.25'
_chemical_formula_weight         813.84
_chemical_name_common            'compound 2.(ca. 1.25H2O)'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.911(1)
_cell_length_b                   14.533(1)
_cell_length_c                   16.558(1)
_cell_measurement_reflns_used    6643
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      2.4
_cell_volume                     3347.5(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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega and phi 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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30258
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.37
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.050
_exptl_absorpt_correction_T_max  0.62
_exptl_absorpt_correction_T_min  0.33
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS, V2.05'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_description       prism
_exptl_crystal_F_000             1624.4
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.361
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.019(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         7273
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+8.6240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0723
_reflns_number_gt                6697
_reflns_number_total             7273
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0393527si20031216_065615_2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C27 H38.50 B Ir N6 O10.25'
_cod_database_code               4112233