Synthesis, Crystal Structure, and H/D Exchange of the Inside Protonated Form of the Cage Imine 4,8,12-Triaza-1-azoniatricyclo[6.6.3.24,12]nonadec-1(15)-ene. A Model for Proton Transfer through an Aliphatic Membrane
Johan Springborg; Bente Nielsen; Carl Erik Olsen; Inger Søtofte; Journal of the American Chemical Society 124 (2002) 5084–5090; doi:10.1021/ja0127638

data_4114778
_publ_section_title
;
 Synthesis, Crystal Structure, and H/D Exchange of the Inside Protonated
 Form of the Cage Imine
 4,8,12-Triaza-1-azoniatricyclo[6.6.3.24,12]nonadec-1(15)-ene. A Model for
 Proton Transfer through an Aliphatic Membrane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5084
_journal_page_last               5090
_journal_paper_doi               10.1021/ja0127638
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C15 H32 Br4 N4 O Zn'
_chemical_formula_weight         669.46
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                86.88(3)
_cell_angle_beta                 88.04(3)
_cell_angle_gamma                85.24(3)
_cell_formula_units_Z            2
_cell_length_a                   8.914(2)
_cell_length_b                   10.946(2)
_cell_length_c                   11.207(2)
_cell_measurement_temperature    120(2)
_cell_volume                     1087.6(4)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement
'Siemens SHELXTL PC version 5.3 (Sheldrick, 1994)'
_computing_structure_solution
'Siemens SHELXTL PC version 5.3 (Sheldrick, 1994)'
_diffrn_ambient_temperature      120(2)
_diffrn_measurement_device       'Siemens SMART CCD Platform'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7603
_diffrn_reflns_theta_max         29.52
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count no
_diffrn_standards_interval_time  no
_diffrn_standards_number         no
_exptl_absorpt_coefficient_mu    8.488
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick. 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.044
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.724
_refine_diff_density_min         -2.144
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.050
_refine_ls_goodness_of_fit_obs   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         5346
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.050
_refine_ls_restrained_S_obs      1.104
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_obs          0.0482
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+4.7720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1208
_refine_ls_wR_factor_obs         0.1108
_reflns_number_observed          4114
_reflns_number_total             5346
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0127638.cif
_cod_data_source_block           JA0127638-33-350
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'no' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+4.7720P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+4.7720P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1087.7(4)
_cod_database_code               4114778