Insights into the Free-Energy Dependence of Intramolecular Dissociative Electron Transfers
Sabrina Antonello; Marco Crisma; Fernando Formaggio; Alessandro Moretto; Ferdinando Taddei; Claudio Toniolo; Flavio Maran; Journal of the American Chemical Society 124 (2002) 11503–11513; doi:10.1021/ja0263644

data_4115161
_publ_section_title
;
 Insights into the Free-Energy Dependence of Intramolecular Dissociative
 Electron Transfers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11503
_journal_page_last               11513
_journal_paper_doi               10.1021/ja0263644
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C19 H21 F2 N O5'
_chemical_formula_weight         381.37
_chemical_name_systematic
; 
 N-(3,6-difluorophtaloyl)-cis-1-aminocyclohexane-4-carboxylate
 tert-butyl perester 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 102.52(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.489(2)
_cell_length_b                   6.0480(10)
_cell_length_c                   24.052(4)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      12
_cell_volume                     1915.5(8)
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'PARST96 (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Philips PW1100 diffractometer'
_diffrn_measurement_method       '\q-2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2930
_diffrn_reflns_theta_full        60.01
_diffrn_reflns_theta_max         60.01
_diffrn_reflns_theta_min         3.36
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_count 50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       prism
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.0015(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     245
_refine_ls_number_reflns         2835
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0775
_refine_ls_shift/su_max          0.530
_refine_ls_shift/su_mean         0.136
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1846P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2271
_refine_ls_wR_factor_ref         0.2435
_reflns_number_gt                1998
_reflns_number_total             2835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0263644_s2_3.cif
_cod_data_source_block           1c
_cod_original_cell_volume        1915.5(5)
_cod_database_code               4115161