Concurrent N-H and α-C-H Bond Activations of Pyrrolidine and Piperidine under Ambient Conditions by 18e Tungsten Allyl Nitrosyl Complexes
Jenkins Y. K. Tsang; Chikako Fujita-Takayama; Miriam S. A. Buschhaus; Brian O. Patrick; Peter Legzdins; Journal of the American Chemical Society 128 (2006) 14762–14763; doi:10.1021/ja065663g

data_4111112
_publ_section_title
;
 Concurrent N-H and \a-C-H Bond Activations of Pyrrolidine and Piperidine
 under Ambient Conditions by 18e Tungsten Allyl Nitrosyl Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14762
_journal_page_last               14763
_journal_paper_doi               10.1021/ja065663g
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C25 H44 N2 O W'
_chemical_formula_weight         572.47
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.560(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7760(10)
_cell_length_b                   18.681(2)
_cell_length_c                   13.0480(10)
_cell_measurement_reflns_used    9031
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.83
_cell_measurement_theta_min      2.17
_cell_volume                     2597.4(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker X8 APEX'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            60650
_diffrn_reflns_theta_full        28.09
_diffrn_reflns_theta_max         28.09
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    4.464
_exptl_absorpt_correction_T_max  0.328
_exptl_absorpt_correction_T_min  0.237
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       prism
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.909
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         6277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0201
_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^)+(0.0182P)^2^+3.5034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0502
_reflns_number_gt                5602
_reflns_number_total             6277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065663gsi20060804_020528.cif
_cod_data_source_block           pl297
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4111112