Iridafurans by Coupling of Alkynes and Aldehydes on a TpMe2Ir System. Facile Demethoxycarbonylation of a β-CO2Me Substituent
Cristóbal, Crispín; García-Rubín, Silvia; Hernández, Yohar A.; López-Serrano, Joaquín; Paneque, Margarita; Posadas, Cristina M.; Poveda, Manuel L.; Rendón, Nuria; Álvarez, Eleuterio; Organometallics 29 (2010) 5744–; doi:10.1021/om1006853

data_4066877
_publ_section_title
;
 Iridafurans by Coupling of Alkynes and Aldehydes on a TpMe2Ir System.
 Facile Demethoxycarbonylation of a \b-CO2Me Substituent
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5744
_journal_paper_doi               10.1021/om1006853
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C29 H36 B Ir N6 O6'
_chemical_formula_sum            'C29 H36 B Ir N6 O6'
_chemical_formula_weight         767.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 104.3480(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0250(3)
_cell_length_b                   8.2245(2)
_cell_length_c                   25.8801(5)
_cell_measurement_reflns_used    8238
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.61
_cell_volume                     3098.33(12)
_computing_cell_refinement       'Bruker (2006). APEX 2. Version 2.1.'
_computing_data_collection       'Bruker (2006). APEX 2. Version 2.1.'
_computing_data_reduction        'Bruker (2006). APEX 2. Version 2.1.'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2003)'
_computing_publication_material  'XCIF, SHELXTL v. 6.14 (Bruker, 2003)'
_computing_structure_refinement  'XL, SHELXTL v. 6.14 (Bruker, 2003)'
_computing_structure_solution    'Bruker (2006). APEX 2. Version 2.1.'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
;
 Bruker-Nonius X8kappa APEX II CCD area detector'
;
_diffrn_measurement_method       'phi and omega scans 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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            38946
_diffrn_reflns_theta_full        30.61
_diffrn_reflns_theta_max         30.61
_diffrn_reflns_theta_min         2.86
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.360
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.2443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS: Area-Detector Absorption Correction. Bruker-AXS
 within v. 7.06 a (Bruker AXS, 2003).
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.743
_refine_diff_density_min         -1.363
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         9491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+2.8603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0673
_reflns_number_gt                8054
_reflns_number_total             9491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1006853_si_001.cif
_cod_data_source_block           1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3098.33(11)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4066877