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_4113454
_publ_contact_author_address
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 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
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 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 H40 B Ir N6 O9, (C2H5OC2H5)'
_chemical_formula_sum            'C37 H50 B Ir N6 O10'
_chemical_formula_weight         941.84
_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
_cell_angle_alpha                86.748(2)
_cell_angle_beta                 85.128(2)
_cell_angle_gamma                76.649(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8078(10)
_cell_length_b                   11.2313(11)
_cell_length_c                   16.667(2)
_cell_measurement_temperature    296(2)
_cell_volume                     1959.9(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_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  0.1157
_diffrn_reflns_av_sigmaI/netI    0.2894
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13539
_diffrn_reflns_theta_max         32.42
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    3.470
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.352
_refine_diff_density_min         -2.670
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.831
_refine_ls_goodness_of_fit_obs   0.976
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         10481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.831
_refine_ls_restrained_S_obs      0.976
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_obs          0.0572
_refine_ls_shift/esd_max         2.025
_refine_ls_shift/esd_mean        0.072
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1301
_refine_ls_wR_factor_obs         0.1037
_reflns_number_observed          5026
_reflns_number_total             10481
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0290375-3_s1_4.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1959.9(3)
_cod_database_code               4113454