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_4078943
_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_formula_moiety         'C23 H31 I3 N6 O2 Rh2'
_chemical_formula_sum            'C23 H31 I3 N6 O2 Rh2'
_chemical_formula_weight         1010.06
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-02-29
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.174(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4283(3)
_cell_length_b                   12.2666(3)
_cell_length_c                   11.9217(3)
_cell_measurement_reflns_used    8440
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      30.8196
_cell_measurement_theta_min      2.9681
_cell_volume                     1516.18(7)
_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      200.00(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_details
;
  1 omega  -97.00   23.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.0970  -19.0000   30.0000 120

  2 omega  -11.00   52.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.0970   38.0000 -150.0000 63

  3 omega   55.00   97.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7220 -178.0000  -30.0000 42

  4 omega  -20.00   27.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.0970  -99.0000  -90.0000 47

  5 omega -103.00  -55.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.0970  178.0000 -150.0000 48

  6 omega  -11.00   58.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7220   38.0000 -120.0000 69

  7 omega  -63.00   49.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7220  -77.0000   90.0000 112
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0143767000
_diffrn_orient_matrix_UB_12      0.0136751000
_diffrn_orient_matrix_UB_13      0.0578334000
_diffrn_orient_matrix_UB_21      0.0481649000
_diffrn_orient_matrix_UB_22      -0.0410149000
_diffrn_orient_matrix_UB_23      0.0057322000
_diffrn_orient_matrix_UB_31      0.0463572000
_diffrn_orient_matrix_UB_32      0.0383906000
_diffrn_orient_matrix_UB_33      -0.0144166000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21203
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.89
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    4.173
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69668
_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 orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.293
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         4649
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+2.2260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0936
_reflns_number_gt                3580
_reflns_number_total             4649
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300569w_si_002.cif
_cod_data_source_block           8_(str1320)
_cod_original_cell_volume        1516.17(6)
_cod_database_code               4078943
_chemical_oxdiff_formula         'C23 H31 N6 O2 I3 Rh2'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22