Synthesis of a Square-Planar Rhodium Alkylidene N-Heterocyclic Carbene Complex and Its Reactivity Toward Alkenes
Palacios, Laura; Miao, Xiaowei; Di Giuseppe, Andrea; Pascal, Simon; Cunchillos, Carmen; Castarlenas, Ricardo; Pérez-Torrente, Jesús J.; Lahoz, Fernando J.; Dixneuf, Pierre H.; Oro, Luis A.; Organometallics 30 (2011) 5208–; doi:10.1021/om2005782

data_4065138
_publ_section_title
;
 Synthesis of a Square-Planar Rhodium Alkylidene N-Heterocyclic Carbene
 Complex and Its Reactivity Toward Alkenes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5208
_journal_paper_doi               10.1021/om2005782
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C52 H57 Cl N2 P Rh'
_chemical_formula_sum            'C52 H57 Cl N2 P Rh'
_chemical_formula_weight         879.33
_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                 91.0910(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6180(10)
_cell_length_b                   23.4030(10)
_cell_length_c                   16.2660(10)
_cell_measurement_reflns_used    78866
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.332
_cell_measurement_theta_min      1.807
_cell_volume                     4421.9(5)
_computing_cell_refinement       'HKL2000(Z. Otwinowski and W. Minor,1997)'
_computing_data_collection       'DENZO (Z. Otwinowski)'
_computing_data_reduction        'HKL2000(Z. Otwinowski and W. Minor,1997)'
_computing_molecular_graphics    'ORTEP (L. Farrugia, 1997) '
_computing_publication_material  'WingX (L. Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.835
_diffrn_measurement_details
' 1.00 degrees, 1.0 sec, detector distance 63.50 mm'
_diffrn_measurement_device_type  'Single-axis HUBER diffractometer'
_diffrn_measurement_method       'fi scans'
_diffrn_radiation_monochromator  'A Si111 double-crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_wavelength     0.73780
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            163452
_diffrn_reflns_reduction_process
;
 Two different orientations of the same crystal(changing 
 pseudokappa 40&#x00BA;)were measured to ensure the data completeness.
 
 Data from the two measurements were corrected for absorption effects,
 scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         33.34
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.513
_exptl_absorpt_correction_T_max  0.9650
_exptl_absorpt_correction_T_min  0.9316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.128
_refine_diff_density_min         -1.679
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.0321(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         12781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1118P)^2^+1.4954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1494
_refine_ls_wR_factor_ref         0.1543
_reflns_number_gt                11427
_reflns_number_total             12781
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2005782_si_001.cif
_cod_data_source_block           compound_2
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4065138