Coupling of Aromatic Aldehydes with CO2Me-Substituted TpMe2Ir(III) Metallacyclopentadienes
Roa, Arián E.; Salazar, Verónica; López-Serrano, Joaqu\?ín; Oñate, Enrique; Alvarado-Rodr\?íguez, José G.; Paneque, Margarita; Poveda, Manuel L.; Organometallics 31 (2012) 3185–; doi:10.1021/om3000554

data_4078047
_publ_section_title
;
 Coupling of Aromatic Aldehydes with CO2Me-Substituted TpMe2Ir(III)
 Metallacyclopentadienes
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              3185
_journal_paper_doi               10.1021/om3000554
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C38 H45 B Ir N7 O13'
_chemical_formula_weight         1010.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 105.232(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   40.649(5)
_cell_length_b                   11.7275(14)
_cell_length_c                   17.870(2)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     8219.6(17)
_computing_cell_refinement       'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_data_collection       'apex2 v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.14 (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 8.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Bruker APEX II DUO 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  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35762
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.43
_diffrn_reflns_theta_min         1.04
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.322
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4064
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.763
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         11447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+2.6676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0663
_reflns_number_gt                9212
_reflns_number_total             11447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3000554_si_002.cif
_cod_data_source_block           enriquen11
_cod_original_cell_volume        8219.3(17)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4078047