Two-Step Synthesis of Hexaammonium Triptycene: An Air-Stable Building Block for Condensation Reactions to Extended Triptycene Derivatives
Michael Mastalerz; Stefanie Sieste; Mila Cenić; Iris M. Oppel; Journal of Organic Chemistry 76 (2011) 6389–6393; doi:10.1021/jo200843v

data_4026482
_publ_section_title
;
 Two-Step Synthesis of Hexaammonium Triptycene: An Air-Stable Building
 Block for Condensation Reactions to Extended Triptycene Derivatives
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6389
_journal_page_last               6393
_journal_paper_doi               10.1021/jo200843v
_journal_volume                  76
_journal_year                    2011
_chemical_formula_sum            'C23 H15 N7 O13'
_chemical_formula_weight         597.42
_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                92.220(2)
_cell_angle_beta                 109.872(3)
_cell_angle_gamma                97.000(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7248(3)
_cell_length_b                   10.2761(3)
_cell_length_c                   13.0872(3)
_cell_measurement_reflns_used    15845
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.4976
_cell_measurement_theta_min      2.9130
_cell_volume                     1216.29(6)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 8.4171
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans, 1453 frames, 15 sec per frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29500
_diffrn_reflns_theta_full        26.25
_diffrn_reflns_theta_max         26.25
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_description       prism
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         4902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0533P)^2^+0.8646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                4334
_reflns_number_total             4902
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo200843v_si_001.cif
_cod_data_source_block           p-1
_cod_database_code               4026482