New mechanistic insights into the copper catalyzed ring expansion of vinyl aziridines: evidence in support of a copper(i) mediated pathway
Mack, Daniel J.; Njardarson, Jon T.; Chemical Science 3 (2012) 3321–; doi:10.1039/c2sc21007j

data_1515249
_publ_section_title
;
 New mechanistic insights into the copper catalyzed ring expansion of
 vinyl aziridines: evidence in support of a copper(i) mediated pathway
;
_journal_issue                   11
_journal_name_full               'Chemical Science'
_journal_page_first              3321
_journal_paper_doi               10.1039/c2sc21007j
_journal_volume                  3
_journal_year                    2012
_chemical_formula_moiety         'C8 H20 N +, C15 H3 F18 Ni O6 -, 0.5 C6 H14'
_chemical_formula_sum            'C26 H30 F18 N Ni O6'
_chemical_formula_weight         853.22
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                83.547(3)
_cell_angle_beta                 90.332(3)
_cell_angle_gamma                70.468(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9155(6)
_cell_length_b                   10.9991(6)
_cell_length_c                   15.6366(9)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      26.84
_cell_measurement_theta_min      2.18
_cell_volume                     1595.32(16)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEXII DUO CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube with Miracol optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            81970
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.756
_exptl_absorpt_correction_T_max  0.9561
_exptl_absorpt_correction_T_min  0.5520
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             862
_exptl_crystal_size_max          0.89
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.070
_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     502
_refine_ls_number_reflns         7908
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0247P)^2^+2.8243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                6539
_reflns_number_total             7908
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2sc21007j.txt
_cod_data_source_block           jtn102
_cod_database_code               1515249