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_1515250
_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 O6 Zn -'
_chemical_formula_sum            'C23 H23 F18 N O6 Zn'
_chemical_formula_weight         816.79
_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   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.056(2)
_cell_angle_beta                 80.156(2)
_cell_angle_gamma                67.947(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3786(13)
_cell_length_b                   10.8425(14)
_cell_length_c                   15.1786(19)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.84
_cell_measurement_theta_min      2.34
_cell_volume                     1559.8(3)
_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    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker Kappa APEXII DUO CCD diffractometer'
_diffrn_measurement_method       '\f and \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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33132
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.934
_exptl_absorpt_correction_T_max  0.8962
_exptl_absorpt_correction_T_min  0.4201
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             816
_exptl_crystal_size_max          1.12
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         11353
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0513P)^2^+0.3996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                8896
_reflns_number_total             11353
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2sc21007j.txt
_cod_data_source_block           jtn103
_cod_database_code               1515250