Divalent Dirhodium Imido Complexes: Formation, Structure, and Alkyne Cycloaddition Reactivity
Shin Takemoto; Shohei Otsuki; Yasuhiro Hashimoto; Ken Kamikawa; Hiroyuki Matsuzaka; Journal of the American Chemical Society 130 (2008) 8904–8905; doi:10.1021/ja8033922

data_4108063
_publ_section_title
;
 Divalent Dirhodium Imido Complexes: Formation, Structure, and Alkyne
 Cycloaddition Reactivity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8904
_journal_page_last               8905
_journal_paper_doi               10.1021/ja8033922
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C40 H45 N Rh2'
_chemical_formula_weight         745.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 92.249(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.763(4)
_cell_length_b                   16.265(7)
_cell_length_c                   16.571(6)
_cell_measurement_temperature    293(2)
_cell_volume                     3437(2)
_computing_cell_refinement       'rigaku process auto'
_computing_data_collection       'rigaku process auto'
_computing_data_reduction        'rigaku process auto'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'rigaku raxis rapid'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1297
_diffrn_reflns_av_sigmaI/netI    0.1156
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32560
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_T_max  0.9902
_exptl_absorpt_correction_T_min  0.5448
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   abscor
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       sheet
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.848
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.431
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         7864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.431
_refine_ls_R_factor_all          0.1543
_refine_ls_R_factor_gt           0.1013
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2629
_refine_ls_wR_factor_ref         0.2837
_reflns_number_gt                4723
_reflns_number_total             7864
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8033922-file002.cif
_cod_data_source_block           shelxl
_cod_database_code               4108063