GaCl~3~-Catalyzed Insertion of Diazene Derivatives into the Cyclopropane Ring
Vadim S. Korotkov; Oleg V. Larionov; Anja Hofmeister; Jörg Magull; Armin de Meijere; Journal of Organic Chemistry 72 (2007) 7504–7510; doi:10.1021/jo0704816

data_4024187
_publ_contact_author
;
 Prof. Dr. Armin de Meijere
 Institut fuer Organische und Biomolekulare Chemie
 Universitaet Goettingen
 Tammannstr. 2
 37077 Goettingen
 Bundesrepublik Deutschland
;
_publ_contact_author_email       armin.demeijere@chemie.uni-goettingen.de
_publ_contact_author_fax         +49(0)551-39-9475
_publ_contact_author_phone       +49(0)551-39-3232
_publ_section_title
;
 GaCl~3~-Catalyzed Insertion of Diazene Derivatives into the
 Cyclopropane Ring
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7504
_journal_page_last               7510
_journal_paper_doi               10.1021/jo0704816
_journal_volume                  72
_journal_year                    2007
_chemical_formula_sum            'C22 H21 N3 O6'
_chemical_formula_weight         423.42
_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                67.507(8)
_cell_angle_beta                 74.357(9)
_cell_angle_gamma                72.459(9)
_cell_formula_units_Z            2
_cell_length_a                   8.9223(10)
_cell_length_b                   11.0696(12)
_cell_length_c                   11.9651(14)
_cell_measurement_temperature    133(2)
_cell_volume                     1025.0(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10683
_diffrn_reflns_theta_full        24.76
_diffrn_reflns_theta_max         24.76
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.101
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             444
_refine_diff_density_max         0.150
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                2463
_reflns_number_total             3486
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo0704816-File003.cif
_cod_data_source_block           vk217
_cod_database_code               4024187