Synthesis and crystal structure of the bromide salt of the inside protonated form of the cage amine [(2.3)3]adamanzane, 1,4,8,12-tetraazatricyclo[6.6.3.24,12]nonadecane and synthesis of the bowl amine [(2.3)2.21]adamanzane, 1,5,9,12-tetraazabicyclo[7.5.2]hexadecane
Springborg, Johan; Nielsen, Bente; Olsen, Carl Erik; Søtofte, Inger; Journal of the Chemical Society, Perkin Transactions 2  (1999) 2701–; doi:10.1039/a906244k

data_7213161
_publ_section_title
;
 Synthesis and crystal structure of the bromide salt of the inside
 protonated form of the cage amine [(2.3)3]adamanzane,
 1,4,8,12-tetraazatricyclo[6.6.3.24,12]nonadecane and synthesis of the
 bowl amine [(2.3)2.21]adamanzane,
 1,5,9,12-tetraazabicyclo[7.5.2]hexadecane
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              2701
_journal_paper_doi               10.1039/a906244k
_journal_year                    1999
_chemical_formula_sum            'C15 H39 Br N4 O4'
_chemical_formula_weight         419.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           158
_symmetry_space_group_name_Hall  'P 3 -2"c'
_symmetry_space_group_name_H-M   'P 3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            4
_cell_length_a                   8.5328(12)
_cell_length_b                   8.5328(12)
_cell_length_c                   33.241(7)
_cell_measurement_temperature    120(2)
_cell_volume                     2096.0(6)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            30274
_diffrn_reflns_theta_max         34.02
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    1.986
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_F_000             896
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.096
_refine_ls_goodness_of_fit_obs   1.153
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         5233
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.549
_refine_ls_restrained_S_obs      1.760
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_obs          0.0695
_refine_ls_shift/esd_max         0.126
_refine_ls_shift/esd_mean        0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+5.6506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1622
_refine_ls_wR_factor_obs         0.1333
_reflns_number_observed          3406
_reflns_number_total             5234
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            906244ksup1.cif
_cod_data_source_block           9/06244K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+5.6506P] 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^)+(0.0376P)^2^+5.6506P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               7213161