General Approach to Nitrogen-Bridged Bicyclic Frameworks by Rh-Catalyzed Formal Carbenoid Insertion into an Amide C-N Bond.
Harada, Shingo; Kono, Masato; Nozaki, Tomoyuki; Menjo, Yasuhiro; Nemoto, Tetsuhiro; Hamada, Yasumasa; The Journal of organic chemistry 80 (2015) 10317–10333; doi:10.1021/acs.joc.5b01954

data_4031554
_publ_section_title
;
 General Approach to Nitrogen-Bridged Bicyclic Frameworks by Rh-Catalyzed
 Formal Carbenoid Insertion into an Amide C-N Bond.
;
_journal_issue                   20
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              10317
_journal_page_last               10333
_journal_paper_doi               10.1021/acs.joc.5b01954
_journal_volume                  80
_journal_year                    2015
_chemical_formula_moiety         'C16 H25 N O6'
_chemical_formula_sum            'C16 H25 N O6'
_chemical_formula_weight         327.38
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                90.206(4)
_cell_angle_beta                 103.919(3)
_cell_angle_gamma                115.144(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6378(5)
_cell_length_b                   10.0839(5)
_cell_length_c                   10.0864(5)
_cell_measurement_reflns_used    3662
_cell_measurement_temperature    93
_cell_measurement_theta_max      68.22
_cell_measurement_theta_min      4.55
_cell_volume                     855.05(8)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9248
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             352.00
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.290
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3060
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0521P)^2^+0.3301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1223
_reflns_number_gt                2394
_reflns_number_total             3060
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo5b01954_si_003.cif
_cod_data_source_block           141202harada
_cod_depositor_comments
'Adding full bibliography for 4031554--4031556.cif.'
_cod_original_cell_volume        855.05(7)
_cod_database_code               4031554