Substituted Diazatetracyclo[4.4.0.13,10.15,8]dodecanes as Stable Caged Proton Sponges
Juraj Galeta; Milan Potáček; Journal of Organic Chemistry 77 (2012) 1010–1017; doi:10.1021/jo202235f

data_4026900
_publ_section_title
;
 Substituted Diazatetracyclo[4.4.0.13,10.15,8]dodecanes as Stable Caged
 Proton Sponges
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1010
_journal_page_last               1017
_journal_paper_doi               10.1021/jo202235f
_journal_volume                  77
_journal_year                    2012
_chemical_formula_sum            'C66 H98 Cl6 N8 O4'
_chemical_formula_weight         1280.22
_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                81.534(3)
_cell_angle_beta                 74.721(3)
_cell_angle_gamma                80.600(3)
_cell_formula_units_Z            2
_cell_length_a                   12.5909(5)
_cell_length_b                   16.0545(6)
_cell_length_c                   16.6187(6)
_cell_measurement_temperature    120(2)
_cell_volume                     3177.8(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26241
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  0.9086
_exptl_absorpt_correction_T_min  0.8808
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.424
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         11153
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0638
_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^)+(0.1126P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.1880
_reflns_number_gt                6207
_reflns_number_total             11153
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo202235f_si_005.cif
_cod_data_source_block           gj634
_cod_database_code               4026900