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_4078043
_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_moiety         'C35 H40 B Ir N6 O6, O0.5 C2 H5'
_chemical_formula_sum            'C37 H45 B Ir N6 O6.5'
_chemical_formula_weight         880.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 115.4760(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.2080(9)
_cell_length_b                   20.8774(10)
_cell_length_c                   22.3156(11)
_cell_measurement_reflns_used    9846
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     8078.7(7)
_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 0.999
_diffrn_measured_fraction_theta_max 0.927
_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  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            87963
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.59
_diffrn_reflns_theta_min         1.40
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.356
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.740
_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            orange
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             3544
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         5.522
_refine_diff_density_min         -2.987
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     947
_refine_ls_number_reflns         21028
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0658P)^2^+38.7000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1390
_reflns_number_gt                16588
_reflns_number_total             21028
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3000554_si_002.cif
_cod_data_source_block           enriquen1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C37 H45 B Ir N6 O6.50'
_cod_database_code               4078043