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_4108065
_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            'C37 H56 N2 Rh2'
_chemical_formula_weight         734.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.111(4)
_cell_length_b                   11.438(4)
_cell_length_c                   17.523(4)
_cell_measurement_temperature    296(2)
_cell_volume                     3630.0(17)
_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      296(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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33687
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    0.934
_exptl_absorpt_correction_T_max  0.8351
_exptl_absorpt_correction_T_min  0.7669
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   abscor
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.45(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         8249
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.0734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0597
_reflns_number_gt                7384
_reflns_number_total             8249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8033922-file004.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        3629.7(16)
_cod_database_code               4108065