Radical Multicomponent Carboamination of [1.1.1]Propellane.
Kanazawa, Junichiro; Maeda, Katsuya; Uchiyama, Masanobu; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b11865

data_4126779
_publ_section_title
;
 Radical Multicomponent Carboamination of [1.1.1]Propellane.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b11865
_journal_year                    2017
_chemical_formula_moiety         'C17 H28 N2 O6'
_chemical_formula_sum            'C17 H28 N2 O6'
_chemical_formula_weight         356.41
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-08-30 deposited with the CCDC.
2017-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.19
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.965
_cell_length_b                   10.523
_cell_length_c                   19.478
_cell_measurement_reflns_used    19430
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.39
_cell_measurement_theta_min      2.17
_cell_volume                     1980.176
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'EAGER 16M'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_wavelength     0.72932
_diffrn_reflns_av_R_equivalents  0.0985
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19430
_diffrn_reflns_theta_full        31.39
_diffrn_reflns_theta_max         31.39
_diffrn_reflns_theta_min         2.17
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.095
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.133(8)
_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   1.050
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         5492
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0675
_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^)+(0.1157P)^2^+0.2458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1812
_reflns_number_gt                5076
_reflns_number_total             5492
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7b11865_si_002.cif
_cod_data_source_block           004-2017c-007_jka203-095a
_cod_original_cell_volume        1980.2
_cod_database_code               4126779
_olex2_refinement_description
;
;
_olex2_date_sample_data_collection 2017-06-26
_olex2_date_sample_submission    2017-07-21
_olex2_submission_original_sample_id 004-2017C-007_JKA203-095A
_olex2_submission_special_instructions 'No special instructions were received'