Facile Oxidative Addition of N-C and N-H Bonds to Monovalent Rhodium and Iridium
Oleg V. Ozerov; Chengyun Guo; Vyacheslav A. Papkov; Bruce M. Foxman; Journal of the American Chemical Society 126 (2004) 4792–4793; doi:10.1021/ja049659l

data_4112472
_publ_section_title
;
 Facile Oxidative Addition of N-C and N-H Bonds to Monovalent Rhodium and
 Iridium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4792
_journal_page_last               4793
_journal_paper_doi               10.1021/ja049659l
_journal_volume                  126
_journal_year                    2004
_chemical_absolute_configuration unk
_chemical_compound_source
;
?
;
_chemical_formula_sum            'C54 H86 Cl2 N2 P4 Rh2'
_chemical_formula_weight         1163.88
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             04-04-03
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.339(2)
_cell_length_b                   13.873(2)
_cell_length_c                   32.296(6)
_cell_measurement_reflns_used    14
_cell_measurement_temperature    294
_cell_measurement_theta_max      12
_cell_measurement_theta_min      10
_cell_volume                     5976.4(17)
_computing_cell_refinement
; 
 Cad4 Express, (Straver, 1992)  
;
_computing_data_collection
; 
 Enraf-Nonius CAD4 
;
_computing_data_reduction
; 
MolEN (Fair, 1990) 
;
_computing_molecular_graphics
; 
 CAMERON (Watkin et al 1996) 
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2003) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2003) 
;
_computing_structure_solution
; 
 SIR92 (Altomare et al, 1994) 
;
_diffrn_ambient_temperature      294
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
; 
Unknown 
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.05
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            9638
_diffrn_reflns_theta_full        23.292
_diffrn_reflns_theta_max         23.768
_diffrn_reflns_theta_min         3.295
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
; 
 Azimutal absorption correction (North et al, 1968) 
;
_exptl_crystal_colour            ' dark green '
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       ' prism '
_exptl_crystal_F_000             2420
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.29
_refine_diff_density_max         2.09
_refine_diff_density_min         -1.46
_refine_ls_abs_structure_details 'Flack, 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.01(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1685
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         3790
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2245
_refine_ls_R_factor_gt           0.0888
_refine_ls_shift/su_max          0.002700
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 2.29 -2.68 1.16 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1332
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0497
_reflns_limit_h_max              15
_reflns_limit_h_min              0
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              36
_reflns_limit_l_min              -36
_reflns_number_gt                3790
_reflns_number_total             9060
_reflns_threshold_expression     I>1.96u(I)
_cod_data_source_file            ja049659lsi20040305_114557.cif
_cod_data_source_block           Determination_D2_rev1
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        ' C27 H41.50 Cl1 N1 P2 Rh1 '
_cod_database_code               4112472