Decarbonylation of Aliphatic Aldehydes by a TpMe2Ir(III) Metallacyclopentadiene
Roa, Arián E.; Salazar, Verónica; López-Serrano, Joaquín; Oñate, Enrique; Paneque, Margarita; Poveda, Manuel L.; Organometallics 31 (2012) 716–; doi:10.1021/om201094q

data_4068108
_publ_section_title
;
 Decarbonylation of Aliphatic Aldehydes by a TpMe2Ir(III)
 Metallacyclopentadiene
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              716
_journal_paper_doi               10.1021/om201094q
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety
'C28 H36 B1 Ir1 N6 O9, 0.5xC4 H10 O1, 0.4 C1 H2 Cl2'
_chemical_formula_sum            'C30.4 H41.8 B Cl0.8 Ir N6 O9.5'
_chemical_formula_weight         874.67
_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                78.0530(10)
_cell_angle_beta                 84.7740(10)
_cell_angle_gamma                69.8550(10)
_cell_formula_units_Z            4
_cell_length_a                   10.9591(5)
_cell_length_b                   15.4387(7)
_cell_length_c                   23.2626(11)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.3
_cell_volume                     3614.2(3)
_computing_cell_refinement       'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_data_collection       'apex2 v. 4.0 (Bruker AXS, 2008)'
_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 8.26
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            45253
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.84
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.813
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.7289
_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
v. 2008.1 (2008) 
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             1751
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.734
_refine_diff_density_min         -1.473
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     932
_refine_ls_number_reflns         17154
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+4.7844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0743
_reflns_number_gt                14108
_reflns_number_total             17154
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201094q_si_002.cif
_cod_data_source_block           enrique28as
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C30.40 H41.80 B Cl0.80 Ir N6 O9.50'
_cod_database_code               4068108