Y-Shaped Tris-N-Heterocyclic-Carbene Ligand for the Preparation of Multifunctional Catalysts of Iridium, Rhodium, and Palladium
Gonell, Sergio; Poyatos, Macarena; Mata, José A.; Peris, Eduardo; Organometallics 31 (2012) 5606–; doi:10.1021/om300569w

data_4078942
_publ_section_title
;
 Y-Shaped Tris-N-Heterocyclic-Carbene Ligand for the Preparation of
 Multifunctional Catalysts of Iridium, Rhodium, and Palladium
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              5606
_journal_paper_doi               10.1021/om300569w
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration unk
_chemical_formula_moiety
'0.5(C21 H26 I3 Ir N6 Pd), 0.5(C21 H28 I3 Ir N6 Pd), C2 H3 N'
_chemical_formula_sum            'C23 H30 I3 Ir N7 Pd'
_chemical_formula_weight         1083.84
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-03-26
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.107(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2740(5)
_cell_length_b                   16.7105(4)
_cell_length_c                   14.4848(5)
_cell_measurement_reflns_used    11799
_cell_measurement_temperature    199.95(10)
_cell_measurement_theta_max      29.4388
_cell_measurement_theta_min      2.7815
_cell_volume                     3053.84(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      199.95(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_details
;
  1 omega  -10.00   15.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.2816  -57.0000 -120.0000 25

  2 omega  -86.00  -59.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.2816  178.0000  -30.0000 27

  3 omega  -12.00   24.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.2816  -99.0000 -180.0000 36

  4 omega    5.00   82.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9847   37.0000  -60.0000 77

  5 omega  -13.00   14.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9847  -99.0000  120.0000 27

  6 omega  -11.00   88.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9847   37.0000 -150.0000 99

  7 omega  -74.00  -39.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.2816  133.0000   33.0000 35

  8 omega  -67.00   46.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9847  -77.0000 -120.0000 113
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0303617000
_diffrn_orient_matrix_UB_12      -0.0149543000
_diffrn_orient_matrix_UB_13      -0.0288136000
_diffrn_orient_matrix_UB_21      0.0432001000
_diffrn_orient_matrix_UB_22      -0.0069528000
_diffrn_orient_matrix_UB_23      0.0425694000
_diffrn_orient_matrix_UB_31      -0.0192871000
_diffrn_orient_matrix_UB_32      -0.0391229000
_diffrn_orient_matrix_UB_33      0.0034123000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0743
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35772
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.50
_diffrn_reflns_theta_min         2.79
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    7.999
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1996
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.209
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.189
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         14702
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0074P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0525
_refine_ls_wR_factor_ref         0.0582
_reflns_number_gt                11831
_reflns_number_total             14702
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300569w_si_002.cif
_cod_data_source_block           of_3_(str1328)
_cod_original_cell_volume        3053.83(17)
_cod_database_code               4078942
_chemical_oxdiff_formula         'C21 H28 N6 I3 In Pd'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32