N-Heterocyclic Carbene-Amide Rhodium(I) Complexes: Structures, Dynamics, and Catalysis
Busetto, Luigi; Cassani, M. Cristina; Femoni, Cristina; Mancinelli, Michele; Mazzanti, Andrea; Mazzoni, Rita; Solinas, Gavino; Organometallics 30 (2011) 5258–; doi:10.1021/om200631w

data_4065231
_publ_contact_author
;
Dr. Andrea Mazzanti
University of Bologna
Department of Organic Chemistry A.Mangini
Viale Risorgimento 4
40136 Bologna
Italy
;
_publ_section_title
;
 N-Heterocyclic Carbene-Amide Rhodium(I) Complexes: Structures, Dynamics,
 and Catalysis
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5258
_journal_paper_doi               10.1021/om200631w
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C29 H34 Cl N3 O3'
_chemical_formula_weight         508.04
_chemical_name_common            'compound 1c'
_chemical_name_systematic
; 
 3-(2-((tert-butoxycarbonyl)amino)ethyl)-1-trityl-1H-imidazol-3-ium chloride 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             10/10/2010
_audit_creation_method           SHELXL-97
_audit_update_record             06/12/2011
_cell_angle_alpha                90.00
_cell_angle_beta                 93.2710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5286(9)
_cell_length_b                   17.0903(18)
_cell_length_c                   18.910(2)
_cell_measurement_temperature    296(2)
_cell_volume                     2751.8(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27780
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  0.9034
_exptl_absorpt_correction_T_min  0.8741
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.60
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.7505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                4693
_reflns_number_total             5416
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200631w_si_001.cif
_cod_data_source_block           g41
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4065231