Metallacarbenes from Diazoalkanes: An Experimental and Computational Study of the Reaction Mechanism
Revital Cohen; Boris Rybtchinski; Mark Gandelman; Haim Rozenberg; Jan M. L. Martin; David Milstein; Journal of the American Chemical Society 125 (2003) 6532–6546; doi:10.1021/ja028923c

data_4113763
_publ_section_title
;
 Metallacarbenes from Diazoalkanes: An Experimental and Computational
 Study of the Reaction Mechanism
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6532
_journal_page_last               6546
_journal_paper_doi               10.1021/ja028923c
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C20 H35 N P2 Rh'
_chemical_formula_weight         454.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 112.08(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.628(4)
_cell_length_b                   10.970(2)
_cell_length_c                   20.463(4)
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      2.73
_cell_volume                     4499.0(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_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  0.0710
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4762
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    0.904
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       prism
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         4762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+1.8015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0652
_reflns_number_gt                3881
_reflns_number_total             4762
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja028923csi20030124_101934.cif
_cod_data_source_block           m312
_cod_original_cell_volume        4499.0(16)
_cod_database_code               4113763