Syntheses, Conformations, and Basicities of Bicyclic Triamines
Thomas W. Bell; Heung-Jin Choi; William Harte; Michael G. B. Drew; Journal of the American Chemical Society 125 (2003) 12196–12210; doi:10.1021/ja030236d

data_4114215
_publ_section_title
;
 Syntheses, Conformations, and Basicities of Bicyclic Triamines
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12196
_journal_page_last               12210
_journal_paper_doi               10.1021/ja030236d
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C12 H24 I N3'
_chemical_formula_weight         339.14
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2b'
_symmetry_space_group_name_H-M   'P b c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.867(11)
_cell_length_b                   13.898(12)
_cell_length_c                   11.504(15)
_cell_measurement_temperature    293(2)
_cell_volume                     2217(4)
_computing_cell_refinement       'Stoe Software'
_computing_data_collection       'Stoe Software'
_computing_data_reduction        'Stoe Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Stoe Stadi 2circle diffractometer'
_diffrn_measurement_method       'variable width w scan'
_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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.1102
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2370
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 20
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    2.126
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.342
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_F_000             1360
_refine_diff_density_max         1.52
_refine_diff_density_min         -0.75
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2370
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.172
_refine_ls_R_factor_gt           0.084
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/[\s^2^(Fo^2^)+(0.003i*Fo^2)]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.086
_refine_ls_wR_factor_ref         0.177
_reflns_number_gt                1329
_reflns_number_total             2370
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            ja030236d_2.cif
_cod_data_source_block           12HI
_cod_depositor_comments
;
The symmetry lines in the original file correspond to space group
'P c 21 b'. With them, the displayed structure is chemically impossible.
Replacing these lines with those corresponding to the group indicated by
the authors in the _symmetry_space_group_name_H-M tag (P b c 21), the structure
becomes reasonable. Hence, the space group has been kept as P b c 21
and the symmetry lines have been changed accordingly. The symmetry lines in
the original file were:
* 'x, y, z'
* '-x, y+1/2, -z'
* 'x, y+1/2, -z+1/2'
* '-x, y, z+1/2'
The Z value has been also fixed to get the real formula of the compound.

Miguel.

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.003i*Fo^2)]' 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^)+(0.003i*Fo^2)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2988(6)
_cod_original_formula_sum        'C12 H24 I N3    '
_cod_database_code               4114215