Highly Selective Intramolecular Carbene Insertion into Primary C-H Bond of α-Diazoacetamides Mediated by a (p-Cymene)ruthenium(II) Carboxylate Complex
Vanessa Kar-Yan Lo; Zhen Guo; Matthew Kwok-Wai Choi; Wing-Yiu Yu; Jie-Sheng Huang; Chi-Ming Che; Journal of the American Chemical Society 134 (2012) 7588–7591; doi:10.1021/ja3006989

data_4117908
_publ_contact_author_address
;
Department of Chemistry
The University of Hong Kong
Pokfulam Road, Pokfulam,
Hong Kong SAR, 
P. R. CHINA
;
_publ_contact_author_email       cmche@hku.hk
_publ_contact_author_fax         '(852)2915 5176'
_publ_contact_author_name        'Professor C. M. Che'
_publ_contact_author_phone       '(852)2859 2153'
_publ_section_title
;
 Highly Selective Intramolecular Carbene Insertion into Primary C-H Bond
 of \a-Diazoacetamides Mediated by a (p-Cymene)ruthenium(II) Carboxylate
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7588
_journal_page_last               7591
_journal_paper_doi               10.1021/ja3006989
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C51 H52 Cl N O5 Ru'
_chemical_formula_sum            'C51 H52 Cl N O5 Ru'
_chemical_formula_weight         895.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.420(1)
_cell_angle_beta                 69.503(1)
_cell_angle_gamma                62.713(1)
_cell_formula_units_Z            2
_cell_length_a                   13.3535(12)
_cell_length_b                   13.8763(13)
_cell_length_c                   15.4248(14)
_cell_measurement_reflns_used    13343
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.64
_cell_volume                     2249.5(4)
_computing_cell_refinement       'SAINT v7.34A (Bruker AXS Inc, 2006)'
_computing_data_collection       'SMART (Bruker AXS Inc, 2004)'
_computing_data_reduction
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2006)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\w scan'
_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  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13343
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.64
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.455
_exptl_absorpt_correction_T_max  0.9516
_exptl_absorpt_correction_T_min  0.8318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         7795
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+1.0929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                6668
_reflns_number_total             7795
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja3006989_si_003.cif
_cod_data_source_block           wt1505w-shelxl
_cod_database_code               4117908